<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 23rd March 2026? Check out new documents from the field of spectroscopy/spectrometry and related techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>LECO,</strong> <strong>Shimadzu </strong>and <strong>Waters Corporation</strong> and brochure by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. LECO: Determination of Nitrogen in Fertilizer</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/CN_FP_928_NITROGEN_FERTILIZERS_203_821_615_4d4b013a08.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Nitrogen is one of the most important elements for plant development and is the macronutrient that is most often found to be deficient in arable soils used for crop production. Nitrogen plays a key role in the formation of enzymes and proteins, which promotes lush, vigorous growth and development in plants that often leads to an increase in the yield from the plant. Fertilizers are utilized to re-introduce nitrogen back into arable soils. Fertilizers can be grouped by their makeup and/or origins into categories including inorganic and/or synthetic (including nitrates, ammonium, and urea) and organic (including compost materials and manures). The accurate and precise determination of nitrogen in all fertilizer types is not only important in the process of blending and preparing the fertilizer material for use, but also will have significant impact on the commercial value and guarantee of the fertilizer.&nbsp;</p><p>The CN928/FP928 is a macro combustion carbon and nitrogen/protein determinator that utilizes a pure oxygen environment in a high-temperature horizontal ceramic combustion furnace designed to handle macro sample mass. A thermoelectric cooler removes moisture from the combustion gases before they are collected in a ballast. The gases equilibrate and mix in the ballast before a representative aliquot (3 cm<sup>3</sup> or 10 cm<sup>3</sup> volume) of the gas is extracted and introduced into a flowing stream of inert gas (helium or argon) for analysis. The aliquot gas is carried to a thermal conductivity cell (TC) for the detection of nitrogen (N<sub>2</sub>).</p><h4><strong>Instrument Model and Configuration&nbsp;</strong></h4><p>Thermal conductivity detectors work by detecting changes in the thermal conductivity of the analyte gas compared to the constant thermal conductivity of the reference/carrier gas. The greater the difference between the thermal conductivity of the carrier gas and the analyte gas, the greater the sensitivity of the detector. The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=24&amp;search=CN928"><strong>CN928</strong></a>/<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=24&amp;search=FP928"><strong>FP928</strong></a> supports either the use of helium or argon as the instrument's carrier gas. When used as a carrier gas, helium provides the highest sensitivity, and the best performance at the lower limit of the nitrogen range. The thermal conductivity difference between argon and nitrogen is not as great as the thermal conductivity difference between helium and nitrogen, therefore the detector is inherently less sensitive when using argon as a carrier gas.</p><h4><strong>TYPICAL RESULTS&nbsp;</strong></h4><p>Data was generated utilizing a single standard, forced through origin calibration using ~ 0.1 g of NIST 913b Uric Acid (33.23% N). Alternatively, LECO 503-530 LCRM Urea may be used for calibration.</p><h3><strong>2. Shimadzu: Evaluation of Microscopic Foreign Matter in Recycled Plastics Using Dynamic Image Analysis, Infrared Microscopy, and SEM-EDS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00861_en_7485baba21.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User Benefits</strong></h4><ul><li>&nbsp;It is easy to evaluate the size and quantity of microscopic foreign particles, which are key quality criteria of recycled plastics.</li><li>With the microcell method of DIA, microscopic foreign matter can be detected and counted quickly using a small sample quantity.</li><li>Infrared microscope and SEM-EDS systems provide information about the morphology and composition of microscopic foreign matter that is useful for improving recycling processes.</li></ul><p>One of the quality criteria for recycled plastic flakes and pellets is the content of foreign matter. Quantitatively evaluating the size and quantity of foreign particles contained in flakes and pellets is important for examining foreign matter removal processes intended to improve pellet quality and optimize manufacturing processesfor products made with recycled materials.&nbsp;</p><p>In this article, pellets of virgin and recycled polyethylene terephthalate (hereafter PET) were dissolved in hexafluoro-2-propanol (hereafter HFIP), a solvent for dissolving PET, to prepare suspensions of insoluble microscopic foreign particles. These suspensions were measured with a dynamic particle image analysis (DIA) system (<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=iSpect+DIA-10"><strong>iSpect DIA-10</strong></a>) to evaluate the size and number of insoluble microscopic foreign particles (patent pending). In addition, part of the suspensions were diluted tenfold and filtered through a membrane filter to collect the insoluble microscopic foreign particles on the filter. The morphology and composition of the collected microscopic foreign particles were evaluated using a digital microscope, an infrared microscope system (<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=IRTracer-100"><strong>IRTracer-100</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=AIM-9000"><strong>AIM-9000</strong></a>), and an SEM-EDS system. These evaluations enabled comparison of the sizes, quantities, and types of foreign particles contained in virgin and recycled materials.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>By using an iSpect DIA-10 system to measure suspensions prepared by dissolving two types of PET pellets (virgin and recycled) in HFIP, we obtained particle images of insoluble foreign matter and evaluated size and concentration of particles. That enabled quantitative comparison of particle size and count in microscopic foreign matter contained in virgin and recycled materials.&nbsp;</p><p>In addition, after diluting the pellet suspensions, the insoluble microscopic foreign matter in the diluted suspensions was collected on filters. The morphology and composition of the microscopic foreign matter were evaluated using an infrared microscope and SEM-EDS system. The results indicated that the suspensions contained organic substances, such as cellulose and amide-based compounds, and inorganic substances and metals that contain elements such as C, O, Ca, and Al (suggestive of carbonates and metallic aluminum).&nbsp;</p><p>Thus, the iSpect DIA-10 enables simple quantitative evaluation of the size and number of microscopic foreign particles in PET pellets using only small sample quantities. Furthermore, composition evaluation by infrared microscope and SEM-EDS systems provides useful information for investigating the origin of foreign matter, examining measures to reduce foreign matter, and evaluating impacts on final products. If similarities in size and shape are observed, particle images obtained with iSpect DIA-10 can also potentially be used to estimate particle composition.</p><h3><strong>3. Thermo Fisher Scientific: Ensuring safer and effective pharmaceutical formulations by X-ray diffraction</strong></h3><ul><li>Brochures and specifications</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PF_41381_xrd_solutions_pharma_9b89684165.pdf"><strong>Full PDF for download</strong></a></li></ul><p>From drug discovery and preformulation studies to the efficient scaling up in the manufacturing process in the plant and finally through QA/QC validation, X-ray diffraction (XRD) is a vital analysis method in the characterization of different physico-chemical properties of the active pharmaceutical ingredient (API). XRD is a gold standard method and required technique in the determination of polymorphic and salt screening, % of crystallinity and stability/reactivity studies of the final API.&nbsp;</p><h5><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2297"><strong>Thermo Scientific™ SolstiX™ XRD Software</strong></a><strong> with Security Suite extends ARL EQUINOX 100 X-ray Diffractometers to 21 CFR Part 11 regulated labs&nbsp;</strong></h5><ul><li>Protect stored electronic data related to quality assurance within manufacturer’s computer systems&nbsp;</li><li>Put controls in place to keep records authentic, incorruptible, and confidential&nbsp;</li><li>Electronic signatures for the user to take responsibility for the electronic data in the system&nbsp;</li><li>Requirements in the data record: date and time of scan, name of the unique signer, and technological controls to ensure security (e.g. passwords)&nbsp;</li></ul><h5><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2143"><strong>Thermo Scientific™ ARL™ EQUINOX 100 X-ray benchtop diffractometer</strong></a><strong> is designed to exceed your analytical needs&nbsp;</strong></h5><ul><li>Ideally suited for rapid screening of various formulations, finger printing or detection of counterfeit products&nbsp;</li><li>Polymorphism and crystallinity determination, crystallite size calculation, quantitative phase analysis, reactivity and stability of materials, etc.&nbsp;</li><li>XRD experiments on standard powders, bulks, tablets, small quantities, etc.&nbsp;</li><li>Real-time full pattern XRD based on our unique PSD detector technology&nbsp;</li><li>X-ray source based on micro-source technology with no external water cooling</li><li>Unique dual-mode capability: reflection and/or transmission&nbsp;</li></ul><h5><strong>Thermo Scientific™ ARL™ EQUINOX 100 XRD for structural analysis&nbsp;</strong></h5><ul><li>Easy-to-use simultaneous full pattern XRD based on unique real time PSD detector technology&nbsp;</li><li>Unique dual-mode capability on a benchtop XRD instrument: reflection and/or transmission mode&nbsp;</li><li>XRD experiments on various samples with sample spinner, capillary stage, sample changer or in controlled environment</li></ul><h5><strong>Top XRD benefits for pharma&nbsp;</strong></h5><ul><li>Structural characterization technique&nbsp;</li><li>Nondestructive technique&nbsp;</li><li>Small amount of sample needed for analysis&nbsp;</li><li>Unique diffraction patterns and quick response&nbsp;</li><li>Analysis on mixtures as well as amorphous content&nbsp;</li><li>Easy determination of induced structural changes</li></ul><h3><strong>4. Waters Corporation: SIMI: A Different Approach to Revealing Dangerous Subvisible Impurities</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009094_en_fb955e89ec.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Foreign particulate matter, also known as extrinsic particles, has become a serious threat to patient safety in recent years, with cases linked to severe immunogenic reactions, deaths, and costly recalls.<sup>1</sup> In 2021 alone, Takeda recalled 1.6 million doses of the Moderna COVID-19 mRNA vaccine in Japan after several patient deaths were linked to steel particulates shed from a malfunctioning pump.<sup>2</sup> Over the span of seven years, from 2014–2017, there were more than 110 drug recalls as a result of glass delamination,<sup>3–4</sup> and several more due to remnant crystals,<sup>5</sup> owing to the difficulty of identifying the presence and source of foreign particulate matter. To prevent against such threats, manufacturers require high throughput technologies to better identify foreign particulate matter in real time.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>Shining a Light on Extrinsic Particles with SIMI</strong></h5><p>Side illumination membrane imaging (SIMI) is a proprietary illumination, imaging, and analysis technique exclusively available to <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2190"><strong>Aura instruments</strong></a>. Utilizing the principles of darkfield microscopy,<sup>6</sup> SIMI is conducted on an Aura membrane plate using an oblique illumination source which emits light at an angle parallel to the surface of the plate.&nbsp;</p><p>Compared to backgrounded membrane imaging (BMI), which utilizes brightfield microscopy (epi-illumination) where particles scatter the incident light isotropically (i.e., at all angles), side illumination membrane maging (SIMI) is a technique that is specifically designed to detect light scattering from high refractive index particles, as well as those that protrude out of the plane from the membrane surface. A particle’s average SIMI intensity is measured in a relative scale where the inherent SIMI scattering of the membrane is defined as SIMI = 0. Positive SIMI values indicate particles protruding out of the membrane, as is the case with microplastics, fibers, and other common extrinsic particles, whose average SIMI intensities vary from 0–255. On some occasions, like with metallic particles and absorbing oils, particles will have reduced light refraction relative to the membrane and thus display negative SIMI values, varying from 0 to -122.&nbsp;</p><p>The majority of foreign, extrinsic particles exhibit a high refractive index and are mechanically rigid in structure, causing them to protrude from the membrane surface and scatter side illumination to a high degree, ideal for SIMI analysis. In contrast, biologic particles exhibit the opposite properties—low refractive index and malleable structures, causing them to lie flat with minimal side scatter profiles, which is best analyzed with BMI or fluorescence membrane microscopy (FMM). Utilizing all three microscopy approaches is most ideal to facilitate the determination of all extrinsic (non-biologic) and inherent (biologic) particles in biologic formulations.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>SIMI is a unique approach to providing additional characterization of subvisible particles and is available in all Aura models to help rapidly identify foreign material in biological samples with a high degree of specificity. A key tertiary imaging mode in addition to BMI and FMM, SIMI provides selective, orthogonal morphological information to identify tall and rigid materials, a defining feature of most extrinsic particles (Figure 11). While particle sizing and counting is done via BMI, SIMI provides illumination, imaging, and analysis that can be useful across a variety of biological products to reveal foreign subvisible particles from the earliest to the latest of stages in the bioprocess.</p>

News from LabRulezICPMS Library - Week 13, 2026

<p><strong>This study investigates the chemical transformations of Eugenia uniflora essential oil under thermal conditions simulating gas chromatography analysis. GC–MS and NMR revealed that sesquiterpenes of the germacrene type, such as furanodiene, undergo sigmatropic rearrangement to form elemene-type compounds, including curzerene.</strong></p><p>Thermal treatment confirmed the formation of rearrangement products, indicating that bioactive properties historically attributed to curzerene may instead originate from furanodiene. The findings highlight the importance of combining complementary analytical techniques, such as NMR, to avoid misinterpretation of essential oil composition and bioactivity markers.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c08966"><strong>Is Curzerene Responsible for the Bioactive Properties of Eugenia uniflora? A Possible Misinterpretation of Bioactive Markers</strong></a></h4><p>Vinicius Monteiro Schaffka, Raphaela Pereira Guaringue, Larissa Kozan, André Luis Kerek, Cássia Gonçalves Magalhães, Andersson Barison, and Barbara Celânia Fiorin*</p><p>ACS Omega 2025, 10, 48, 59425–59434</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c08966">https://doi.org/10.1021/acsomega.5c08966</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><div><p>Essential oils are a matrix of volatile and complex compounds characterized by strong odors and significant biological activity. In plants, they play a crucial role in defense against bacteria, viruses, and predators. <a href="javascript:void(0);">(1)</a> These biological properties support the extensive use of essential oils in the food, cosmetics, and pharmaceutical industries. <a href="javascript:void(0);">(1,2)</a> <i>Eugenia uniflora</i> L., commonly known as pitangueira, is a native Brazilian tree widely distributed across South America and is well-known for its bioactive essential oil. <a href="javascript:void(0);">(3)</a> Beyond the consumption of its fruits in natura or functional beverages, its leaves are used in infusions, decoctions, and tinctures to treat a variety of diseases, including diarrhea, stomach pain, worm infestations, fever, flu, hyperglycemia, hyperlipidemia, and hypertension. <a href="javascript:void(0);">(4,5)</a> Studies have shown that the composition of secondary metabolites in <i>E. uniflora</i> can vary depending on factors such as fruit color, ripening stage, <a href="javascript:void(0);">(6)</a> and seasonal influences. <a href="javascript:void(0);">(4,7−10)</a></p><p>The essential oil of <i>E. uniflora</i> is predominantly composed of sesquiterpenes, mainly germacrene-type, such as curzerene, germacrene B, germacrone, germacrene D, selina-1,3,7(11)-trien-8-one, and its oxide. Additionally, Elemene-type terpenes are also reported, including furanodiene, β-Elemene, and β-Elemenone. <a href="javascript:void(0);">(11−13)</a></p><p>However, those sesquiterpenes are well-documented for their thermal instability. When heat is applied, germacrene-type sesquiterpenes undergo a [3,3]-sigmatropic rearrangement, known as Cope rearrangement, converting into Elemene-type terpenes as presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c08966#fig1">Figure 1</a>. <a href="javascript:void(0);">(14−16)</a> This reaction is widely utilized as a synthetic pathway to produce Elemenes from germacrene precursors. <a href="javascript:void(0);">(17,18)</a></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_48_59425_59434_Figure_1_3_3_Sigmatropic_rearrangement_of_Germacrene_type_into_Elemene_type_250708e73c.jpg" alt="ACS Omega 2025, 10, 48, 59425–59434: Figure 1. [3,3]-Sigmatropic rearrangement of Germacrene-type into Elemene-type." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_48_59425_59434_Figure_1_3_3_Sigmatropic_rearrangement_of_Germacrene_type_into_Elemene_type_250708e73c.jpg 245w," sizes="100vw" width="3000" height="984"></p><p>Gas chromatography (GC) is the main technique for characterizing essential oils, often coupled with mass spectrometry (GC-MS) and the retention index determination is used in the identification of the compounds through comparison with databases. <a href="javascript:void(0);">(21)</a> During GC analysis, essential oils are subjected to multiple heating stages. Initially, the sample is exposed to a high inlet temperature, typically around 240 °C, to ensure complete volatilization. It then enters the oven, where the temperature follows a programmed ramp starting at 60 °C, increasing at 3 °C/min, and reaching up to 240 °C. Finally, the sample encounters the elevated temperatures of the mass spectrometry (MS) detector’s source (250 °C) and interface (280 °C). Even in isocratic methods, where the oven temperature remains constant throughout the analysis, the inlet, source, and interface temperatures are maintained at high levels. Although the sample passes through these stages briefly, the elevated temperatures can induce Cope rearrangements in the essential oil, leading to possible changes in its composition. <a href="javascript:void(0);">(22,23)</a></p><p>The accurate characterization of the chemical composition of essential oils is crucial for any study employing them as a biological or analytical matrix, as it supports the interpretation of bioactivity, chemotaxonomic classification, and quality control of samples with economic value added. There are many studies attributing relevant biological activities, classifying specimens, and identifying phenotypic and genetic variations based on the chemical composition of the essential oil of <i>E. uniflora</i> L., which is usually characterized by GC-MS. <a href="javascript:void(0);">(8,9,11,24)</a> As an example of the study carried out by de Jesus, found acute anti-inflammatory effect of a rich in curzerene essential oil. <a href="javascript:void(0);">(5)</a> Similarly, Pascoal, reported distinct essential oil composition patterns among <i>E. uniflora</i> varieties─yellow, red, and purple fruits─primarily driven by variations in β-Elemene and germacrene D content. <a href="javascript:void(0);">(7)</a> These findings highlight metabolic changes during fruit ripening and underscore the influence of genetic diversity among <i>E. uniflora</i> varieties. Such exhibitions are unsatisfactory, because they sustain all their evidence in the characterization of their essential oil only by GC-MS analysis, without considering the Cope rearrangements, a fact that may change the outcome of their research. In this context Nuclear Magnetic Resonance (NMR) spectroscopy is a good alternative for essential oil analysis, since is a robust not destructive technique and able to detect and quantify simultaneously a wide range of metabolites that exceed the concentration of about 5–10 μM. <a href="javascript:void(0);">(25)</a></p><p>In order to highlight analytical concerns about the uses of only GC-MS data to access chemical relevance of <i>E. uniflora</i> essential oil studies, Nuclear Magnetic Resonance (NMR) spectroscopy was employed to evaluate the chemical composition of the essential oil of <i>Eugenia uniflora</i> L. before and after an induced thermal treatment, compared to GC-MS data. The findings provide insights into thermolabile compounds and highlight potential misidentifications of the bioactive properties associated with the sesquiterpenes of <i>E. uniflora</i> present in literature.</p><h4><strong>2. Results and Discussion</strong></h4><h5><strong>2.1. Characterization of the Essential Oil</strong></h5><p>Approximately 60 compounds, mostly sesquiterpenes (Germacrene B) and oxygenated sesquiterpenes (Germacrone), were visualized in the essential oil, with the 9 compounds having a relative area above 2%, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c08966#tbl1">Table 1</a>. The identified and most prevalent compounds align with those reported in the literature for <i>E. uniflora</i>. <a href="javascript:void(0);">(4,11,12)</a> It is possible to highlight the significant proportion of Germacrene-type sesquiterpenes compared to Elemene-type, except Curzerene, which was found in high concentration.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_48_59425_59434_Table_1_Main_Components_Identified_in_the_GC_MS_Analysis_of_the_Essential_Oil_from_Leaves_of_E_uniflora_9d59d96bef.jpg" alt="ACS Omega 2025, 10, 48, 59425–59434: Table 1. Main Components Identified in the GC–MS Analysis of the Essential Oil from Leaves of E. uniflora." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_48_59425_59434_Table_1_Main_Components_Identified_in_the_GC_MS_Analysis_of_the_Essential_Oil_from_Leaves_of_E_uniflora_9d59d96bef.jpg 218w," sizes="100vw" width="1076" height="771"></p><p>The variation in the composition of the essential oil from <i>E. uniflora</i> leaves was described in literature, <a href="javascript:void(0);">(9)</a> who classified the specimens into three groups: Group I, containing yellow, dark red, and purple fruits, which showed high concentrations of germacrene B, germacrone, and atractylone; Group II, consisting of light red fruit samples, with high concentrations of curzerene, germacrene D, and germacrene A; and Group III, containing orange-red fruits, with a high content of selina-1,3,7(11)-trien-8-one and oxyselina-1,3,7(11)-trien-8-one. According to this classification, this essential oil fits into Group II.</p><p>Chemical transformations of many components found in the <i>E. uniflora</i> leaves essential oil result from the heating conditions typically applied during GC–MS analysis, which occur through Cope Rearrangement. <a href="javascript:void(0);">(12,19)</a> Cope rearrangement is a stereospecific [3,3]-sigmatropic rearrangement that proceeds via the most stable chairlike transition state of 1,5-cyclodecadiene, from germacrene-type, to give 1,2-divinylcyclohexane, known as Elemene-type. <a href="javascript:void(0);">(14)</a> Some of the Cope rearrangements found in the <i>E. uniflora</i> essential oil are represented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c08966#fig2">Figure 2</a>. <a href="javascript:void(0);">(11,22,23,26)</a></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_48_59425_59434_Figure_2_Cope_Rearrangements_of_sesquiterpenes_7fe9282d75.jpg" alt="ACS Omega 2025, 10, 48, 59425–59434: Figure 2. Cope Rearrangements of sesquiterpenes." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_48_59425_59434_Figure_2_Cope_Rearrangements_of_sesquiterpenes_7fe9282d75.jpg 150w," sizes="100vw" width="1500" height="1566"></p><p>The same essential oil was analyzed using NMR spectroscopy to identify its components. Although NMR identification is considerably more labor-intensive than GC-MS analysis, it offers the advantage of being a cold and nondestructive technique. Since the sample does not undergo heating during the process, its stability is preserved throughout the analysis. The conformational differences observed in germacrene-type compounds further increase the spectrum’s complexity, leading to signal broadening in the <sup>1</sup>H NMR spectra. <a href="javascript:void(0);">(27)</a></p><p>A substantial number of signals were observed in the <sup>1</sup>H spectrum, with the majority concentrated between 0.5 and 3.0 ppm, a region characteristic of terpene compounds. The region between 4.5 and 6.0 ppm also exhibited numerous signals attributed to vinylic protons, observed in sesquiterpenes (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c08966#fig3">Figure 3</a>).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_48_59425_59434_Figure_3_1_H_NMR_400_13_M_Hz_CD_Cl3_spectra_of_the_raw_essential_oil_a46e04574e.jpg" alt="ACS Omega 2025, 10, 48, 59425–59434: Figure 3. 1H NMR (400.13 MHz, CDCl3) spectra of the raw essential oil." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_48_59425_59434_Figure_3_1_H_NMR_400_13_M_Hz_CD_Cl3_spectra_of_the_raw_essential_oil_a46e04574e.jpg 245w," sizes="100vw" width="4175" height="2376"></p><h4><strong>3. Conclusions</strong></h4><p>The investigation of the composition of <i>E. uniflora</i> essential oil by NMR and the thermal treatment performed proved that curzerene may come from furanodiene due to the transformations that occur in the matrix during gas chromatographic analysis. These findings have significant implications for the investigation into the chemical composition of <i>E. uniflora</i> essential oil and the evaluation of the biological properties of its sesquiterpenes. Since each technique has advantages and disadvantages, combining GC-MS analysis with a cold technique, such as NMR is important to guarantee the proper identification of the compound genuinely responsible for any property assigned to <i>E. uniflora</i> essential oil.</p><h4><strong>4. Materials and Methods</strong></h4><h5><strong>4.2. GC-MS Analysis</strong></h5><p>The gas chromatographic analyses of the essential oils (10 mg mL<sup>–1</sup>) were performed using a gas chromatography–mass spectrometry system (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=QP2020"><strong>Shimadzu GCMS-QP2020 Gas Chromatograph</strong></a>). The analyses were conducted on an RTx-5MS capillary column (30 m × 0.25 mm internal diameter × 0.25 μm film thickness), and the analytical conditions were as follows: split ratio of 1/10, injector temperature at 250 °C, ion source at 250 °C, and interface at 280 °C. The temperature program of the oven was set at 60 °C for 5 min, followed by a temperature ramp of 3 °C/min until reaching the final temperature of 240 °C. The components were identified based on the relative retention index, calculated for each constituent by injecting a series of <i>n</i>-alkane standards (C8–C20) under the same sample conditions and comparing them with tabulated values as well as by comparing the obtained mass spectra with the mass spectra database and literature comparisons. <a href="javascript:void(0);">(21)</a></p><h5><strong>4.4. NMR Analysis</strong></h5><p>All NMR spectra were acquired at 298 K on a <strong>Bruker AVANCE III</strong> spectrometer operating at 9.4 T, observing <sup>1</sup>H at 400.13 MHz and <sup>13</sup>C at 100.13 MHz, equipped with a broadband probe. The essential oil was solubilized in CDCl<sub>3</sub> with 0.05% of tetramethylsilane (TMS) used as an internal reference. The <sup>1</sup>H NMR spectra were recorded utilizing 65k time-domain data points across a spectral width of 20.00 ppm. This setup provided a digital resolution of 0.24 Hz. The data were obtained using a single 30° excitation pulse, with a relaxation delay of 1.0 s, and an average of 128 scans. The <sup>13</sup>C NMR spectra was carried out using the <i>zgpg30</i> pulse sequence utilizing 64k time-domain data points across a spectral width of 238 ppm, with an acquisition time of 1.3631 s, providing a digital resolution of 0.7434 Hz and a relaxation delay of 2.0s and an average of 2k scans.</p><p>The HSQC and HMBC experiments were conducted using standard pulse sequences from the Bruker library, with modifications to the number of acquired points to improve resolution, 2048 in F2 and 512 in F1.</p></div>

Is Curzerene Responsible for the Bioactive Properties of Eugenia uniflora? A Possible Misinterpretation of Bioactive Markers

<p><strong>This study investigates how ionization polarity influences the gas-phase stability of native-like proteins analyzed by ion mobility spectrometry–mass spectrometry. While proteins generally retain folded structures in both positive and negative electrospray ionization modes, significant differences in unfolding behavior were observed.</strong></p><p>Proteins exhibited greater gas-phase stability when analyzed in the ionization polarity corresponding to their solution-phase charge, requiring higher energy for unfolding. These findings emphasize the importance of considering protein isoelectric points and ionization polarity in native IMS-MS experiments to ensure accurate structural characterization.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295"><strong>Investigating the Effect of Isoelectric Points on the Gas-Phase Stability of Native-like Proteins Analyzed in Positive- versus Negative-Ion Mode by IMS-MS</strong></a></h4><p>Alexis N. Edwards, Madeline G. Bannon, Michael S. Cordes, and Elyssia S. Gallagher*</p><p>Anal. Chem. 2026, 98, 6, 4518–4527</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acs.analchem.5c04295">https://doi.org/10.1021/acs.analchem.5c04295</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><div><p>In native mass spectrometry (nMS), the native-like structures of proteins are maintained in the gas phase by preserving the secondary, tertiary, and quaternary structures. <a href="javascript:void(0);">(1−7)</a> The preservation of native-like protein structures is primarily accomplished via the use of electrospray ionization (ESI), a soft ionization method that forms a distribution of multiply charged protein ions. These multiply charged ions can then be investigated to characterize stoichiometry, oligomeric composition, and ligand binding. <a href="javascript:void(0);">(8−10)</a></p><p>During ESI, a potential is applied to the sample-containing solution. In an aqueous spray solvent, H<sub>3</sub>O<sup>+</sup> and OH<sup>–</sup> are produced in positive-ion mode (+ESI) and negative-ion mode (−ESI), respectively. <a href="javascript:void(0);">(11)</a> The buildup of like-charges within the solution results in the formation of a Taylor Cone at the capillary tip, which ejects charged droplets that travel toward the inlet of the mass spectrometer. Droplets undergo evaporation and fission until complete analyte desolvation, leading to the release of folded, gas-phase protein ions. As the droplets shrink, H<sub>3</sub>O<sup>+</sup> or OH<sup>–</sup> can become concentrated, causing the pH of the droplet to decrease or increase, respectively. Shifts in pH can denature proteins. Therefore, to maintain native-like protein structures, nMS is conducted with solutions containing volatile salts, usually ammonium acetate, that provide ionic strength and minimize pH changes compared to spraying from pure water. <a href="javascript:void(0);">(11,12)</a> Droplet pH in ESI is influenced by flow rate, solvent composition, and applied voltage, <a href="javascript:void(0);">(13)</a> but often approaches values near the p<i>K</i><sub>a</sub> of acetate (4.76) or ammonium (9.25) in +ESI or −ESI, <a href="javascript:void(0);">(12,14)</a> respectively. During ESI, changes in overall protein charge take place via proton transfer at chargeable amino acid residues, resulting in the formation of protonated or deprotonated protein ions with the charged sites being dependent on the relative proton affinities of ammonium, acetate, and chargeable amino acids as proteins near complete desolvation. <a href="javascript:void(0);">(15−19)</a></p><p>Ion mobility spectrometry (IMS) measures an ion’s mobility through an inert gas under the influence of an electric field. Thus, mobility is directly influenced by the ion’s size, shape, and charge. <a href="javascript:void(0);">(20)</a> A protein’s mobility can be used to estimate its structure by calculating an average momentum-transfer collisional cross section (CCS). In addition to structural characterization, IMS-MS can investigate the gas-phase stability of protein complexes when paired with collision-induced unfolding (CIU). Specifically, in CIU experiments, protein ions are accelerated into a cell filled with inert gas molecules and undergo multiple collisions with higher frequency and energy relative to IMS. This converts kinetic energy to internal, vibrational energy, disrupting noncovalent interactions and inducing unfolding of the protein ions. <a href="javascript:void(0);">(21)</a> Unfolding alters the protein structure, which can then be quantified by monitoring the protein’s mobility during subsequent IMS-MS measurement. <a href="javascript:void(0);">(22)</a> Prior work with mutant proteins has shown that proteins with similar intramolecular interactions have similar CIU fingerprints, while proteins with different intramolecular interactions have different CIU fingerprints. <a href="javascript:void(0);">(23)</a> Therefore, gas-phase protein stability is correlated with intramolecular interactions.</p><p>Past native IMS-MS work has primarily been conducted in +ESI given that -ESI has the reputation of being unreliable for native-like protein analysis due to the occurrence of corona discharge, <a href="javascript:void(0);">(24)</a> and charge-state distributions that may not be representative of folded proteins. <a href="javascript:void(0);">(25)</a> In recent years, −ESI has been increasingly used in CIU and IMS-MS, with recent work demonstrating that −ESI-MS is capable of discerning denatured and native-like protein structures. <a href="javascript:void(0);">(26,27)</a> Prior work showed that charge manipulation of folded proteins, such as charge reduction, to achieve similar absolute charge states in both ion modes, results in CCS values of protein cations that are comparable to their anion counterparts. <a href="javascript:void(0);">(26,28)</a> This suggests that gas-phase structures are weakly dependent on protein charge and ionization polarity. <a href="javascript:void(0);">(23,26,28)</a> Yet, Hong et al. showed that, in the absence of charge reduction, the gas-phase stability of two proteins (avidin and β-lactoglobulin) is sensitive to ionization polarity, highlighting that gas-phase stability is not consistent between +ESI and −ESI. <a href="javascript:void(0);">(29)</a></p><h4><strong>Materials and Methods</strong></h4><h5><strong>Native IMS-MS Analysis</strong></h5><p>Glass capillaries were pulled using a P-1000 micropipette puller (Sutter Instrument Company, Novato, CA). Samples and calibrants were sprayed from pulled capillaries (inner diameter ∼1 μm) and analyzed with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/152"><strong>Synapt G2-S High-Definition MS </strong></a>(Waters Corporation, Milford, MA). The trap and transfer cells contained Ar, the helium cell contained He, and the IMS cell contained N<sub>2</sub>. IMS wave velocity was 350 m/s, while IMS wave height was either 7 or 9 V, depending on the protein size (see <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Table S2</a>). Proteins with larger mass required a wave height of 9 V to ensure that all the ions migrated out of the IMS cell prior to the next ion injection. Mass spectra were collected and signal averaged over 30 s. Additional instrument details can be found in the Supporting Information (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Table S2</a>).</p><p>To limit systematic error due to repositioning of the ESI tip between runs, <a href="javascript:void(0);">(48)</a> the <i>XYZ</i>-stage position was optimized and kept consistent for all replicates. Approximately 5 μL of sample was loaded into a glass capillary, which was then mounted on the <i>XYZ</i>-stage. Electric potential was delivered to the sample by a platinum wire inserted into the capillary and placed in contact with the solution. The voltage applied to the tip holder ranged from 0.60 to 1.2 kV for native samples, and 0.80 to 1.40 kV for denatured samples. Nine replicates in each ion mode were collected for all proteins with measurements spread across 8 days over 3 weeks. These replicates were conducted in pairs by collecting data in both ion modes consecutively. To accomplish this, a CIU experiment was collected in +ESI before the instrument polarity was changed to −ESI. A second CIU experiment was performed, beginning with −ESI to counteract any changes in protein stability due to pH changes during ESI. <a href="javascript:void(0);">(14)</a> This allowed for use of the same capillary, at the same position in relation to the instrument inlet, for each +ESI/–ESI replicate pair. A new tip was used for each +ESI/–ESI replicate pair. CIU experiments were accomplished by increasing collision voltage (CV) to the trap cell in 5 V steps, from 0 V to a maximum of 120 V.</p><h4><strong>Results and Discussion</strong></h4><p>Ten proteins were chosen for analysis in +ESI and −ESI in this work (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#tbl1">Table 1</a>). These proteins can be broken into three groups depending on the net-charge in solution at pH 7: net-negative (with pI &lt; 6.5), net-neutral (with 6.5 ≤ pI ≤ 7.5), and net-positive (with pI &gt; 7.5). Five of the ten proteins have a net-negative charge at pH 7, though four of these proteins (con A, β-lactoglobulin, ovalbumin, and α-lactalbumin) are routinely analyzed via +ESI-IMS-MS. <a href="javascript:void(0);">(18,28)</a> Additionally, each protein had charge-state distributions in +ESI and −ESI that resulted in at least one overlapping charge state (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#fig1">Figure 1</a>), allowing for direct comparison of <sup>TW</sup>CCS<sub>N2→He</sub> and CIU50 in both ion modes.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Anal_Chem_2026_98_6_4518_4527_Figure_1_Representative_mass_spectra_in_ESI_top_and_ESI_bottom_cb81976247.jpg" alt="Anal. Chem. 2026, 98, 6, 4518–4527: Figure 1. Representative mass spectra in +ESI (top) and −ESI (bottom) for (A) ovalbumin, (B) GNA, (C) β-lactoglobulin, (D) α-lactalbumin, (E) con A, (F) streptavidin, (G) ubiquitin, (H) WGA, (I) cytochrome c, and (J) lysozyme. Proteins that have blue or red charge states indicate additional oligomeric states that were detected. Outlines in red boxes are overlapping charge states that are compared herein. *Indicates contaminant peaks." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Anal_Chem_2026_98_6_4518_4527_Figure_1_Representative_mass_spectra_in_ESI_top_and_ESI_bottom_cb81976247.jpg 245w," sizes="100vw" width="1600" height="865"></p><h5><strong>Proteins with Disulfide Bridges are Stable in Both Polarities</strong></h5><p>For both lysozyme and α-lactalbumin, the average <sup>TW</sup>CCS<sub>N2→He</sub> were within experimental uncertainty in +ESI and −ESI for both the initial, folded structures and the final, extended structures (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#tbl2">Table 2</a>). However, the 6+ and 6- ions of lysozyme and α-lactalbumin showed a high resistance to unfolding with &gt;90% of the ions retaining their folded <sup>TW</sup>CCS<sub>N2→He</sub> values even at high CV (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#fig2">Figure 2</a>). Replicate data showed similar trends (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Figure S2</a>). While CCS values provide a description of gas-phase structures, CIU experiments provide information on the stability of the gas-phase protein structures. Furthermore, the number and pattern of disulfide bridges present in antibodies has been characterized by CIU. <a href="javascript:void(0);">(63)</a> Lysozyme and α-lactalbumin both contain the glycosyl hydrolases family 22 (GH22) domain, which has four disulfide bridges that span ∼94% and ∼93% of the amino acid sequence, respectively (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Figure S3</a>). Thus, we hypothesize that rather than effects from protein pI and ionization polarity, the unfolding behavior of these proteins is controlled to a greater extent by the presence of stabilizing disulfide bridges that prevent routine unfolding during collisional activation.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Anal_Chem_2026_98_6_4518_4527_Figure_2_Representative_mobiligrams_showing_arrival_times_for_lysozyme_A_C_and_a_lactalbumin_B_D_0f3d23c3c1.jpg" alt="Anal. Chem. 2026, 98, 6, 4518–4527 - Figure 2. Representative mobiligrams showing arrival times for lysozyme (A, C) and α-lactalbumin (B, D) at low and high CV (blue solid and orange dashed lines, respectively) for +ESI (A, B) and −ESI (C, D). For lysozyme, different values were chosen for the high CV (e.g., 540 eV in +ESI and 480 eV in −ESI) because these were the last analyzed CV where the signal-to-noise ratio (S/N) for the 6 ± ions was greater than 3." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Anal_Chem_2026_98_6_4518_4527_Figure_2_Representative_mobiligrams_showing_arrival_times_for_lysozyme_A_C_and_a_lactalbumin_B_D_0f3d23c3c1.jpg 212w," sizes="100vw" width="1600" height="1178"></p><p>To characterize the stabilizing effect of disulfides, MD simulations were conducted that heat denatured 6+ ions of lysozyme and α-lactalbumin with disulfide bridges either present or removed with the resulting cysteine residues being protonated prior to heating (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Figure S4</a>). Structural changes associated with heat denaturation were characterized by taking the root-mean-square deviation (RMSD) of the heated structures relative to initial, crystal structures. Over ten trials, lysozyme ions possessed an average RMSD of (1.6 ± 0.2) nm when disulfides were present which increased to (3.5 ± 0.5) nm when disulfides were removed. Similarly, the RMSD of α-lactalbumin ions increased from (1.8 ± 0.1) nm when disulfides were present to (3.7 ± 0.3) nm when disulfides were removed, suggesting that the disulfides serve as a barrier to unfolding. This is visually represented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Figure S4C,D</a> where simulated structures of heated lysozyme and α-lactalbumin ions with intact disulfides adopt more condensed configurations relative to those with disulfides removed. In essence, the disulfides “tie” disparate regions of protein together, which serves as a barrier to more thorough unfolding even at a maximum simulated temperature of 900 K, explaining the similarity of <sup>TW</sup>CCS<sub>N2→He</sub> values in +ESI versus −ESI as well as the limited percentage of ions that undergo a change in <sup>TW</sup>CCS<sub>N2→He</sub> upon additional collisional activation.</p><p>WGA has 16 disulfide bridges per monomeric subunit (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#tbl1">Table 1</a>). On average, these disulfides encompass seven amino acids each, with ∼78% the total amino acids in WGA being encompassed by at least one disulfide bridge (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c04295/suppl_file/ac5c04295_si_001.pdf">Figure S3</a>). Compared to lysozyme and α-lactalbumin, the presence of disulfide bridges across small numbers of amino acids enables WGA to unfold with ΔCCS of (370 ± 60) Å<sup>2</sup> and (390 ± 120) Å<sup>2</sup> in +ESI and −ESI, respectively (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c04295#tbl2">Table 2</a>). However, in comparison to the other lectins, GNA and con A, we hypothesize that these disulfide bridges in WGA limit the extent of unfolding, resulting in the extended, <sup>TW</sup>CCS<sub>N2→He</sub> values being within experimental uncertainty in both ion modes.</p><p>To summarize, lysozyme and α-lactalbumin exhibit similar gas-phase behavior in both +ESI and −ESI, with most ions retaining folded structures even under high CV. We hypothesize this resistance to unfolding is largely attributed to their four disulfide bridges, which span over 90% of their sequences and act as stabilizing constraints. MD simulations confirm that removing these disulfides significantly increases structural deviation during heat denaturation, indicating their critical role in maintaining compact configurations. Consequently, the presence of disulfide bridges explains the minimal changes in <sup>TW</sup>CCS<sub>N2→He</sub> and the proteins’ high stability under activation.</p><h4><strong>Conclusions</strong></h4><p>IMS-MS allows for detailed analysis of the structure and stability of native-like proteins in the gas phase. The structure of a protein is dictated by its amino acid sequence and the resulting noncovalent interactions that form the secondary, tertiary, and quaternary structures. Chargeable amino acid residues that are solvent exposed can carry charges leading to the protein having a net-positive, net-negative, or net-neutral charge in solution at physiological pH. Yet, most native IMS-MS analysis is conducted in +ESI, leading to proteins that are net-negative in solution experiencing large swings in their net-charge during the ESI process.</p><p>This work highlights that gas-phase stability of native-like proteins varies with ionization polarity. While CCS values for folded structures are generally comparable between +ESI and −ESI, unfolding energetics differ─net-negative proteins are more stable in −ESI, whereas net-positive proteins are more stable in +ESI. We hypothesize that these differences are due to changes in the intramolecular interactions within cationic and anionic proteins. Therefore, proteins analyzed in the mode opposite to their solution-phase charge may have different gas-phase structures compared to biological systems. For example, proteins that are net-negatively charged in physiological environments (pI &lt; 6.5) are more likely to represent their biological counterparts as gas-phase anions when analyzed in −ESI compared to +ESI, enabling nMS experiments to more closely characterize the structures present in biological systems.</p></div>

Investigating the Effect of Isoelectric Points on the Gas-Phase Stability of Native-like Proteins Analyzed in Positive- versus Negative-Ion Mode by IMS-MS

Quantitative Assessment of Chemical Modifications of Macromolecules through Counterion Measurement

<p><strong>In the week of March 30, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><div><div><div><div><div><div><h5><strong>1. Agilent Technologies: Trace the Threat: Py-GC/MS Workflows for Microplastics Characterization</strong></h5><ul><li>Tu, 31.3.2026 06:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/6025">Registration</a></li></ul><p>Discover advanced approaches for trace micro- and nanoplastics analysis using Py-GC/MS and explore how the Agilent 5977C GC/MSD enhances sensitivity, robustness, and workflow efficiency.</p><h5><strong>2. Thermo Fisher Scientific: FTIR microscopy: Practical guidance for effective sample analysis</strong></h5><ul><li>Tu, 31.3.2026 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/6088">Registration</a></li></ul><p>Join this webinar to gain practical guidance on FTIR microscopy workflows, including measurement modes, sample preparation, parameter optimization and spectral interpretation.</p><h5><strong>3. Bruker: Understanding Polymer Reactions and Degradation with FT-IR and EPR Spectroscopy</strong></h5><ul><li>Tu, 31.3.2026 17:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5996">Registration</a></li></ul><p>Discover how FT-IR and EPR spectroscopy reveal polymer curing kinetics and radical-driven mechanisms—enabling real-time monitoring, degree of cure quantification, and stability studies.</p><h5><strong>4. Technology Networks: Advances in Hydrogen Gas Generation for Sustainable Laboratories</strong></h5><ul><li>Tu, 31.3.2026 17:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5941">Registration</a></li></ul><p>Discover how modern hydrogen gas generators support high-purity GC performance while reducing costs and environmental impact. Learn how on-site generation improves uptime, efficiency, and lab sustainability.</p><h5><strong>5. C&amp;EN: Overcoming Raman Microscopy Challenges in Microplastics and Life Sciences</strong></h5><ul><li>We, 1.4.2026 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/6016">Registration</a></li></ul><p>Learn how O-PTIR spectroscopy overcomes fluorescence limitations in Raman microscopy. Discover simultaneous sub-micron IR and Raman analysis for microplastics, biological samples, and organic materials.</p></div></div></div></div></div></div>

Webinars LabRulezGCMS Week 14/2026

<p><strong>In the week of March 30, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Bruker: MALDI Imaging Becomes IR-resistible: Going Multimodal for Advanced Biomedical Insights</strong></h5><ul><li>Mo, 30.3.2026 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5971">Registration</a></li></ul><p>Explore advanced multimodal imaging with MALDI, QCL-based IR, and fluorescence microscopy to achieve ROI-focused molecular insights in complex tissues.</p><h5><strong>2. Shimadzu Corporation: Environmental PFAS Testing: Introducing Next-Generation Mass Spectrometry Solutions</strong></h5><ul><li>Tu, 31.3.2026 09:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/6026">Registration</a></li></ul><p>Explore advanced PFAS analysis strategies combining LC-MS/MS and MALDI-TOF screening to improve sensitivity, efficiency, and regulatory readiness in environmental testing.</p><h5><strong>3. Tosoh Bioscience: Tosoh Tuesday - Scaling Up from Process Development to GMP Production with Pre-packed Columns</strong></h5><ul><li>Tu, 31.3.2026 15:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/6089">Registration</a></li></ul><p>This webinar will introduce SkillPak™ MAX pre-packed columns and present performance data using TOYOPEARL® Super A, a novel Protein A resin.</p><h5><strong>4. Phenomenex: Recipe for Separation: Crafting Your Perfect HPLC Method</strong></h5><ul><li>We, 1.4.2026 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/6091">Registration</a></li></ul><p>Discover how to properly use and maintain your column to maximize its performance and lifespan.</p>

Webinars LabRulezLCMS Week 14/2026

<p><strong>In the week from March 30, the following webinars await you in the field of atomic and molecular spectroscopy and spectrometry</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Bruker: MALDI Imaging Becomes IR-resistible: Going Multimodal for Advanced Biomedical Insights</strong></h5><ul><li>Mo, 30.3.2026 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5971">Registration</a></li></ul><p>Explore advanced multimodal imaging with MALDI, QCL-based IR, and fluorescence microscopy to achieve ROI-focused molecular insights in complex tissues.</p><h5><strong>2. LECO: Moisture and LOI Determination in Cement, Fly Ash, Gypsum, and Lime</strong></h5><ul><li>Tu, 31.3.2026 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5972">Registration</a></li></ul><p>Learn how TGA supports accurate moisture and LOI determination in cement, fly ash, gypsum, and lime, ensuring quality control and compliance with ASTM methods.</p><h5><strong>3. Thermo Fisher Scientific: FTIR microscopy: Practical guidance for effective sample analysis</strong></h5><ul><li>Tu, 31.3.2026 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/6088">Registration</a></li></ul><p>Join this webinar to gain practical guidance on FTIR microscopy workflows, including measurement modes, sample preparation, parameter optimization and spectral interpretation.</p><h5><strong>4. Bruker: Understanding Polymer Reactions and Degradation with FT-IR and EPR Spectroscopy</strong></h5><ul><li>Tu, 31.3.2026 17:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5996">Registration</a></li></ul><p>Discover how FT-IR and EPR spectroscopy reveal polymer curing kinetics and radical-driven mechanisms—enabling real-time monitoring, degree of cure quantification, and stability studies.</p><h5><strong>5. Agilent Technologies: Fueling Accuracy: ICP-OES Analysis for Organic Biofuel and Renewable Fuel Feedstocks</strong></h5><ul><li>Tu, 31.3.2026 20:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/6043">Registration</a></li></ul><p>This webinar provides a practical overview of setting up ICP-OES instrumentation for organic sample analysis.</p><h5><strong>6. C&amp;EN: Overcoming Raman Microscopy Challenges in Microplastics and Life Sciences</strong></h5><ul><li>We, 1.4.2026 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/6016">Registration</a></li></ul><p>Learn how O-PTIR spectroscopy overcomes fluorescence limitations in Raman microscopy. Discover simultaneous sub-micron IR and Raman analysis for microplastics, biological samples, and organic materials.</p><h5><strong>7. SPECTRO Analytical Instruments: AI-Driven Semiquantitative ICP-OES Analysis: Introducing SPECTRO AI QUANT</strong></h5><ul><li>Th, 2.4.2026 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/6090">Registration</a></li></ul><p>This live webinar introduces an AI-driven approach that streamlines semiquantitative analysis across a wide range of sample types.</p><h5><strong>8. Anton Paar: Extensional Rheology of Polymers: Air Bearing Rheometer Applications</strong></h5><ul><li>Th, 2.4.2026 18:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5800">Registration</a></li></ul><p>Learn why extensional rheology is essential for polymer processing. See real measurements, core concepts, and practical examples, and explore SER and UXF solutions for elongational flow testing.</p><h5><strong>9. Agilent Technologies: Heavy Metal Elements in Food Spices: A Critical Analysis Using ICP-MS and ICP-OES Techniques</strong></h5><ul><li>Th, 2.4.2026 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/6044">Registration</a></li></ul><p>This session discusses techniques for determination of heavy metals in food by ICP-OES and ICP-MS.</p>

Webinars LabRulezICPMS Week 14/2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 30th March 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Thermo Fisher Scientific, </strong>brochure by<strong> Shimadzu </strong>and presentation by<strong> MDCW / LECO!</strong></p><h3><strong>1. Agilent Technologies: Extraction and Analysis of Pesticides from Water by Solid Phase Extraction and GC/MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_extraction_analysis_pesticides_water_gcms_5994_8996en_agilent_28fc35d0e7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Drinking water is defined as water intended for human consumption obtained from different sources. Several guidelines/regulations exist for ensuring that undesirable substances such as pesticides are not present in excessive amounts that may be harmful to human health. These regulations ensure that water intended for human consumption can be consumed safely. In India, the Bureau of Indian Standards (BIS) has set regulatory limits for residual pesticides in drinking water (IS 10500)<sup>1</sup> , packaged drinking water (IS 14543)<sup>2</sup> , and natural mineral water (IS 13428).<sup>3</sup> A total of 26 pesticides are regulated by BIS standards, of which four compounds (monocrotophos, phorate, 2,4-D, and isoproturon) are more suitable for analysis by liquid chromatography.&nbsp;</p><p>EPA Method 525.2 is a general-purpose method for determination of organic compounds in finished drinking water or water from any source or treatment stage.<sup>4</sup> This method is applicable to a range of organic compounds that are partitioned from the water sample onto a C18 organic phase packed in a disk or cartridge. The organic compounds are then eluted using a suitable eluent, concentrated, and analyzed by GC/MS.&nbsp;</p><p>This application note describes the use of EPA Method 525.2 for extraction of pesticide residues at trace levels in water using solid-phase extraction (Agilent Bond Elut C18: Straight barrel cartridges, p/n 12102118) and analysis using Agilent 8890-5977 GC/MS.&nbsp;</p><p>Excellent linearity with R2 &gt; 0.995 was obtained for all pesticides considered for the study. Recoveries were obtained in the range of 80–120% with associated RSDs &lt; 15% at 0.005–0.080 ng/mL level of fortification.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrument parameters</strong></h5><ul><li><strong>GC:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890"><strong>Agilent 8890</strong></a></li><li><strong>Column:</strong> Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=J%26W+HP-5ms"><strong>J&amp;W HP-5ms</strong></a> UI 30 m × 0.25 mm, 0.25 μm&nbsp;</li><li><strong>Carrier Gas:</strong> Helium, constant flow, 1.2 mL/min&nbsp;</li><li><strong>Inlet:</strong> Agilent Multimode Inlet (MMI)</li><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977"><strong>5977 GC/MS</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>A simple, easy, and efficient method based on EPA 525.2 was implemented for the determination of 22 pesticides in water. The method demonstrated good sensitivity, precision, and accuracy, and allows for rapid analysis. The results demonstrate that pesticide residues can be detected below the current maximum residue levels (MRL) required by the BIS specifications. Acceptable recoveries and precision were obtained at concentrations as low as 5 ng/L for all pesticides. The method is ideally suited for use in a regulatory laboratory for the determination of pesticides in surface, drinking, and packaged drinking water.</p><h3><strong>2. MDCW / LECO: Exploring PFAS in Consumer Goods Using GCxGC and High-Resolution Mass Spectrometry</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_3_Alonso_6f61e3ea43.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are widely used in consumer and industrial products due to their unique physicochemical properties, but their persistence and potential health risks have made their detection increasingly important. This study focuses on developing an untargeted analytical approach for screening PFAS and related compounds in consumer goods using advanced chromatographic and mass spectrometric techniques.</p><p>The analytical workflow combines gas chromatography with time-of-flight mass spectrometry (GC-TOFMS) and comprehensive two-dimensional gas chromatography coupled with high-resolution TOFMS (GC×GC-HRTOFMS), using systems such as the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1097"><strong>LECO Pegasus® BTX</strong> </a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/38"><strong>Pegasus® HRT+</strong></a> platforms. Sample introduction is performed via thermal desorption or pyrolysis, enabling analysis of both volatile and complex matrices. High-resolution MS provides accurate mass measurements and elemental composition, which are essential for identifying unknown compounds and reducing matrix interferences.</p><p>In the first case study, anti-fog solutions were analyzed and found to contain a wide range of compounds, including fluorotelomer alcohols and related PFAS species. While GC-TOFMS enabled initial screening, high-resolution TOFMS was necessary to characterize unknown compounds through accurate mass determination and complementary ionization techniques (EI and PCI). This approach allowed tentative structural assignment using external databases, demonstrating the importance of HRMS in identifying compounds not present in standard libraries.</p><p>The second case study focused on chewing gum, a highly complex matrix with diverse chemical constituents and trace-level analytes. The use of GC×GC-HRTOFMS significantly improved chromatographic separation and spectral clarity, enabling detailed profiling of volatile and semi-volatile compounds. A dedicated PFAS screening workflow based on mass defect analysis and spectral filtering was applied, leveraging the characteristic CF₂ patterns of PFAS molecules to simplify data interpretation.</p><p>Despite the complexity of the sample, no PFAS were detected in the chewing gum, its packaging, or the box. Overall, the study demonstrates that combining GC×GC separation, high-resolution mass spectrometry, and advanced data processing tools provides a powerful and reliable strategy for untargeted PFAS screening in complex consumer products, particularly when unknown or emerging contaminants are of concern.</p><h3><strong>3. Shimadzu: Gas Chromatograph Nexis GC-2060</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c184_e056_06c3456516.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=Nexis+GC-2060"><strong>Nexis GC-2060</strong></a> represents a new generation of gas chromatographs, built on over 70 years of GC development and designed to serve as a flexible and future-proof analytical platform. It integrates the concept of <i>Analytical Intelligence</i>, which enables automated system monitoring, troubleshooting, and optimization, helping both experienced and less experienced users achieve reliable and consistent results. The system is highly configurable, supporting up to two injectors, three injection units, and four detectors simultaneously, allowing a single instrument to cover multiple analytical applications.</p><p>A key advantage of the Nexis GC-2060 is its versatility in sample introduction and detection. The Multi-Mode Injection Unit (MMI) supports a wide range of injection techniques, including split/splitless, PTV, direct injection, large-volume injection (LVI), and thermal desorption, significantly reducing the need for complex sample preparation. The system is also equipped with next-generation detectors such as FID and TCD, offering high sensitivity, stability, and linearity, with additional detector options (ECD, FPD, FTD, BID) enabling broad application coverage.</p><p>The instrument is designed to maximize laboratory efficiency and minimize downtime. Features such as tool-free column installation (ClickTek), automated startup/shutdown, Easy sTop maintenance mode, and Clean Pilot for automated column conditioning simplify routine operation and reduce manual intervention. In addition, Eco Idling technology automatically optimizes gas and power consumption during standby, significantly lowering operational costs while maintaining readiness for analysis.</p><p>From an analytical performance perspective, the Nexis GC-2060 delivers excellent reproducibility and sensitivity, supported by advanced autosamplers (e.g., AOC-30) and compatibility with third-party systems. The platform supports hydrogen carrier gas for faster analysis and includes smart gas management features such as automatic gas switching. Its modular design allows seamless integration with various sample preparation systems, autosamplers, and detectors, ensuring adaptability to evolving laboratory needs.</p><p>Overall, the Nexis GC-2060 combines high performance, operational efficiency, and flexibility in a single platform, making it suitable for a wide range of applications, including pharmaceutical analysis, environmental testing, food analysis, and energy-related measurements. Its scalability and continuous software updates ensure long-term usability and alignment with future analytical requirements.</p><h3><strong>4. Thermo Fisher Scientific: Accurate multi-component blast furnace gas analysis maximizes iron production and minimizes coke consumption</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/epm_AN_Iron_Production_Prima_PRO_bd5de98b44.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Over a billion tonnes of iron a year are produced in blast furnaces, representing around 94% of global iron production¹. The blast furnace consists of a large steel stack, lined with refractory brick. Iron ore, coke and limestone are dropped into the top of the furnace and preheated air blown into the bottom through nozzles called ‘Tuyeres’. Iron oxides are reduced in the melting zone, or ‘Bosh’, forming liquid iron (called ‘hot metal’) and liquid slag. These liquid products are drained from the furnace at regular intervals, and the blast furnace will run continuously for several years, until the refractory lining needs replacing.</p><p>Analysis of carbon monoxide (CO) and carbon dioxide (CO₂) give vital information on the efficiency of the reduction processes. Historically, two non-dispersive infrared (NDIR) analyzers were used, one to measure CO, the other CO₂. Additional discrete analyzers were required to monitor oxygen and hydrogen – typically paramagnetic O₂ analyzers and thermal conductivity analyzers for H₂.&nbsp;</p><p>Thermo Scientific™ process mass spectrometers have been widely used for many years for key gas analysis applications in iron and steel plants, including blast furnace, basic oxygen steelmaking, coke oven gas analysis, secondary steel process control, fuel gas analysis and direct reduction iron processes²</p><h4><strong>Process control requirements&nbsp;</strong></h4><p>The advantages of process MS over conventional analysis techniques have been proven over many years in the iron and steel industry. The ability to measure a wide range of components on a single analyzer, coupled with advanced calibration, data transmission, and self-diagnostic software, makes the modern mass spectrometer ideal for integration into the modern plant. On blast furnaces, superior gas analysis is being used to calculate gas efficiency, mass and heat balances, and heat profiles through probe analysis, as well as being an essential tool in the early detection of cooling water leaks and sample system failures.&nbsp;</p><p>Figure 2 shows 64 hours of data from a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2305"><strong>Thermo Scientific™ Prima™ PRO Process MS</strong></a> monitoring the six gases in a blast furnace top gas every 10 seconds. The pulse every 12 hours is generated by an automatic nitrogen blowback from the sample conditioning system, to keep the sample probe clear of particulates.</p><h4><strong>Hydrogen analysis&nbsp;</strong></h4><p>An increase in the hydrogen level in the furnace can indicate a leak from the furnace cooling system, as water dissociates into hydrogen and oxygen in the furnace. This has implications both for plant efficiency and plant safety. Water leaks will lower the furnace temperature, causing heat loss and a consequent increase in fuel consumption. In extreme cases, damage to plant and personnel can be caused by ignition of these hazardous mixtures of explosive gases.&nbsp;</p><p>Figure 4 shows a plot of top gas hydrogen concentration measured by Thermo Scientific process MS over a 24-hour period, with the departure of the measured H2 value from that predicted by the mass balance model indicating a water leak. This leak was caused by the failure of a cooling member, and the furnace was taken off blast for repair. The mass spectrometer’s ability to provide fast, accurate hydrogen analysis removes the need for an additional discrete analyzer.&nbsp;</p><p>Gas composition measurement is particularly important during the end-of-campaign blowdown that takes place prior to rebuilds and relines, because explosive gas mixtures can be generated.&nbsp;</p><h4><strong>Probe analysis&nbsp;</strong></h4><p>The fast analysis provided by MS offers another significant advantage over discrete analyzers—a number of process streams can be analyzed using a single instrument. This is achieved using a fully automated multi-inlet system, designed to switch between sample streams at high speeds with minimal sample flushing times. For example, as well as furnace top gas, the MS can also analyze gases from probes placed above and below the burden (the furnace charge of iron ore, coke and limestone). These are known as above-burden and sub-burden probes and provide valuable information on fuel efficiency, iron conversion and furnace charging. Figure 5 shows a schematic of these two probes; they can be moved across the furnace to build a cross-sectional profile of the furnace.</p><h4><strong>Summary&nbsp;</strong></h4><p>Thermo Scientific process mass spectrometers have been successfully monitoring blast furnace off gas at many of the world’s iron and steel companies for over 30 years. For a blast furnace producing 5,000 tonnes a day, a reduction in coke consumption of just 10 kg per tonne of iron produced provides a payback of over $10,000 a day. Users report that the combination of fast, accurate MS gas analysis for gas efficiency, heat and mass balances and hydrogen analysis, with advanced process control and mathematical modeling, has reduced coke consumption by up to 100 kg per tonne and increased iron production. Upgrading to Prima PRO MS can therefore result in complete installation payback within a few weeks.&nbsp;</p><ul><li>Reduces coke consumption&nbsp;</li><li>Produces consistent quality iron&nbsp;</li><li>Reduces downstream processing costs&nbsp;</li><li>Detects water leaks fast&nbsp;</li><li>Improves thermal control of furnace&nbsp;</li><li>Enables safer operation during blowdown</li></ul>

News from LabRulezGCMS Library - Week 14, 2026

News from LabRulezLCMS Library - Week 14, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 30th March 2026? Check out new documents from the field of spectroscopy/spectrometry and related techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Metrohm,</strong> <strong>Shimadzu, Thermo Fisher Scientific </strong>and <strong>Waters Corporation!</strong></p><h3><strong>1. Metrohm: Quantification of methanol in contaminated spirits</strong></h3><p><strong>Protecting consumers from contaminated beverages</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_rs_056_download_3b37cb883a.pdf"><strong>Full PDF for download</strong></a></li></ul><p>An alarming global trend highlights the serious harm that can result from ingesting illegal, improperly distilled alcohol. Home-distilled spirits prepared using industrial solvents (i.e., wood alcohol) and presented as legitimate alcoholic beverages often contain methanol. Methanol causes blindness and can lead to death when ingested. This has led to fatal consequences around the world [1–3].&nbsp;</p><p>The breaking point for the Czech Republic came in September 2012. The sale of hard liquor was temporarily banned after 20 people died from the consumption of spirits with dangerous levels of methanol [2]. After an exhaustive study using various screening tools, the Czech Republic adopted Raman spectroscopy as the method of choice for identifying and quantifying methanol in contaminated spirits. This Application Note demonstrates how Raman spectroscopy can be employed as an efficient and rapid screening method for samples of rum contaminated with methanol.</p><h4><strong>EXPERIMENT&nbsp;</strong></h4><p>This example study measures commercially available coconut rum that is spiked with methanol in concentrations between 0.33% and 5.36%. The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=220&amp;search=iRaman"><strong>iRaman NxG 785H</strong></a> with a fiber-optic probe is used to collect Raman spectra of the mixtures (Figure 3). Table 1 lists the relevant equipment and instrument settings used for this application study. The peak at around 1000 cm-1 (highlighted by the inlay of Figure 3) visibly increases with increasing concentration of methanol, becoming significant at approximately 1%.</p><h4><strong>CONCLUSION</strong></h4><p>These results validate that Raman spectroscopy can be used for rapid, quantitative screening of dangerous adulterants in alcoholic beverages. This technique can be expanded to investigate adulteration in other media such as food, petroleum, and pharmaceutical drugs [4].</p><h3><strong>2. Shimadzu: Evaluation of Organic Impurities in Lithium Carbonate by TOC Analysis</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01098_en_ec9b3e73fc.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User Benefits</strong></h4><ul><li>TOC analysis enables effective control of organic impurities in lithium carbonate.</li><li>Using the combustion tube kit for high-salt samples can extend the lifespan of the combustion tube and catalyst, reducing maintenance frequency.</li><li>With the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=ASI-L+autosampler"><strong>ASI-L autosampler</strong></a>, multiple samples can be measured automatically, improving throughput and efficiency</li></ul><p>Lithium carbonate (Li2CO3) is an important material used in a wide range of applications in the lithium-ion battery industry. For example, it is used as a lithium source for cathode active material synthesis and electrolyte salt production, as a raw material for oxide-based solid electrolytes, and as a form of lithium commonly recovered in recycling processes.&nbsp;</p><p>Because impurities in lithium carbonate can affect downstream processes and final products, appropriate control is essential. In particular, organic impurities require especially careful attention because they may originate from so many sources, such as solvents and processing aids used during purification, residual organics from manufacturing steps, or contamination introduced during handling and storage.&nbsp;</p><p>Total organic carbon (TOC) analysis offers an effective way to manage such organic impurities in raw materials. This article presents an example of using a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=TOC-L"><strong>Shimadzu TOC-L</strong></a> total organic carbon analyzer (Fig. 1) to evaluate the TOC content of lithium carbonate.</p><h4><strong>TOC Analysis&nbsp;</strong></h4><h5><strong>TOC Analysis Methods&nbsp;</strong></h5><p>Two commonly used methods are available for TOC analysis:&nbsp;</p><p><strong>(1) TC - IC method: </strong>Total carbon (TC) and inorganic carbon (IC) are measured separately, and then TOC is calculated as the difference (TOC = TC – IC).</p><p><strong>(2) NPOC method: </strong>TOC is measured as non-purgeable organic carbon (NPOC). After acidifying the sample to pH &lt; 3, IC is subsequently removed by sparging and the remaining carbon is measured as TC, which is regarded as TOC. The acidification and sparging steps are performed automatically by the instrument.&nbsp;</p><p>For lithium carbonate solutions, the amount of carbonatederived IC is typically very high. As a result, the TC–IC method tends to yield calculated TOC values with a larger relative error. Therefore, the NPOC method isrecommended.</p><p>&nbsp;In lithium carbonate solutions prepared as described above, IC is expected to be present mainly as bicarbonate (HCO<sub>3</sub> <sup>–</sup>) and carbonic acid (H<sub>2</sub>CO<sub>3</sub>). If IC is not fully removed during NPOC pretreatment, the TOC result may be overestimated. Therefore, thorough IC removal is critical for samples with high IC content. For actual samples, sparging parameters, such as sparge gas flow rate and sparge time settings, can be adjusted.&nbsp;</p><h5><strong>Combustion Tube for High-Salt Samples&nbsp;</strong></h5><p>The prepared lithium carbonate solution contains a large amount of salts. When a large number of salt-containing samples are analyzed, salts may accumulate inside the combustion tube, which can lead to catalyst clogging, reduced sensitivity, and poorer repeatability.</p><p>For this analysis, the optional combustion tube for high-salt samples was used, shown in Fig. 2. The high-salt combustion tube has a larger diameter than the standard combustion tube and contains larger catalyst particles to help mitigate saltrelated clogging. Thus, the frequency of combustion tube replacement can be significantly reduced.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this article, TOC analysis was performed for a 10 g/L lithium carbonate solution using a Shimadzu TOC-L total organic carbon analyzer. By measuring TOC in the prepared solution, the TOC content in the lithium carbonate solid was calculated. The results showed good recovery rates in the spike-recovery test and consistent performance was also confirmed during long-term continuous analysis. These findings demonstrate that the TOC-L is a reliable solution for measuring TOC in lithium carbonate and for effective management of organic impurities.&nbsp;</p><p>When applying the NPOC method to lithium salt-containing solutions, careful selection of the acid is essential because salts formed during acidification can affect both data quality and instrument condition. For this example, sulfuric acid is recommended.</p><p>In addition, using the optional combustion tube kit for high-salt samples can extend the lifespan of the combustion tube and catalyst, thereby reducing maintenance frequency. This option is especially helpful for samples with high salt concentrations.&nbsp;</p><p>In addition to lithium carbonate, the TOC-L can also be applied to TOC analysis of lithium hydroxide solutions, determination of water-extractable TOC in recycled black mass, and analytical needs in lithium refining processes based on direct lithium extraction (DLE). With its broad applicability across various upstream materials, recycling streams, and refining processes, the TOC-L supports both quality control and process optimization operations throughout the lithium-ion battery value chain.</p><h3><strong>3. Thermo Fisher Scientific: Evaluating Silicon using Raman Microscopy</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/vib_silicon_analysis_with_raman_microscope_app_note_mcs_an1232_en_11_2024_1887815_web_50639c9148.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Raman spectroscopy is a form of vibrational spectroscopy that probes chemical bonds and molecular structure and is sensitive to small changes in chemical and structural environments. The Raman spectrum of a material is a molecular “fingerprint” that can be used for identification of unknown materials and for characterizing and qualifying expected materials. Since intermolecular effects and lattice vibrations are also detected, it can be used to evaluate crystallinity. Mechanical phenomena such as strain can also be detected from peak shifts in Raman spectra. Raman imaging allows visualization of the distribution of components or changes in physical state across the sample.</p><h4><strong>Silicon in aluminum&nbsp;</strong></h4><p>Silicon is used in alloys with aluminum to increase the strength of lightweight aluminum-based parts. Addition of silicon to aluminum also alters the viscosity of melted aluminum, improving the castability. These alloys typically contain 3% to 25% silicon. While silicon and aluminum can form a eutectic mixture, it is common to have finely dispersed silicon particles throughout the material.¹ The size and distribution of silicon particles can affect the strength of the aluminum.&nbsp;</p><p>One common example of an aluminum product, aluminum foil, is made up of almost pure aluminum (approximately 98.5%) but it does contain small amounts of silicon and iron.² Raman imaging of a piece of aluminum foil reveals small particles of silicon (Figure 1). A <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2237"><strong>Thermo Scientific™ DXR3xi Raman Imaging Microscope </strong></a>was used with a 532 nm laser and a 100X&nbsp;metallurgical objective to collect the Raman imaging data. An area of 408 μm x 208 μm was imaged using an image pixel size of 1 μm. The Raman image, based on the 520 cm-1 peak of silicon, shows the spatial distribution of the particles and image analysis provides size and shape information. In this case, 81&nbsp;silicon particles were identified with a size (area) range of 6-151 μm². This analytical approach may be extrapolated to other types of Si/Al alloy parts.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The importance of silicon as a technologically significant material cannot be overstated. It has properties that make it useful in numerous different types of products. Raman micro-spectroscopy has proven itself an important tool for the assessment of molecular structure and physical states of silicon. Raman images provide a way to observe the spatial distribution of silicon and silicon-containing components, structural variations such as crystallinity, and physical effects such as strain. This note showed a few representative examples to illustrate some of the advantages offered by Raman microscopic analysis of silicon. The coverage is not intended to be comprehensive as there are numerous other areas where the Raman analysis of silicon is currently employed and other opportunities where it could be used. The Thermo Scientific DXR3 Raman Microscope and the Thermo Scientific DXR3xi Raman Imaging Microscope have both been shown to be excellent choices for the Raman analysis of silicon samples.</p><h3><strong>4. Waters Corporation: High-Throughput Detection of Degraded Polysorbate in Biological Formulations with FMM</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009114_en_99c7483d1a.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The FDA requires that all biologic formulations be free of visible particles and has defined allowable levels of subvisible particles (SVPs) larger than 10 µm to ensure the potency, efficiency, and safety of these drug.<sup>1</sup> While most protein drug particle analysis focuses on particles formed due to formulation instability, SVPs formed through the degradation of formulation excipients must also be considered.&nbsp;</p><p>Polysorbates 20 (PS20) and 80 (PS80), best known as Tween-20 and -80, are excipients used in &gt;70% of marketed parenteral biological drugs to improve product stability and shelf life.<sup>2</sup> However, when these formulations are stored for long periods of time (&gt;6 months) at low temperatures (4 °C), visible and subvisible particles are formed due to the enzymatic hydrolysis of the polysorbates by host cell proteins (HCPs) such as esterases and lipases.<sup>3,4</sup> PS20 in particular has been found to be extremely prone to degrading into fatty acid particles.<sup>5</sup> Lauric, myristic and palmitic acids are the most common fatty acid degradation products, and there is a direct correlation between low fatty acid solubility and particle formation in common formulation buffers.<sup>3–7</sup> However, high-throughput, sensitive, and specific analysis of polysorbate particles has been difficult due to their complex chemistry and their low concentrations (&lt;&lt;0.5%) in high protein concentration (&gt;100–200 mg/mL) formulation environments, making it a perennial needle in a haystack problem.</p><p>In this application note, we introduce the Aura™ polysorbate degradation assay, a specific and quantitative assay that detects free fatty acid particles (FFAs) formed during polysorbate degradation on Aura PTx System. The assay analyzes 96 samples using anywhere from 5 µL–10 mL of sample in a few hours. <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2190"><strong>Aura™ Systems</strong></a> use backgrounded membrane imaging (BMI) and fluorescence membrane microscopy (FMM) to count, size and ID particles from 1 µm to 5 mm. Fluorescent labels utilized by FMM are selected based on thier ability to interact with particles of a certain nature, allowing for the generation of key information related to identity of the particles.</p><h4><strong>Results and Discussion&nbsp;</strong></h4><h5><strong>Morphological Appearance of Different Fatty Acid Particles&nbsp;</strong></h5><p>Aura systems image every particle, enables subvisible particle size distributions analysis, and makes morphological differentiation possible using built-in image analysis filters. When we analyze different free fatty acid solutions with Aura PTx System, we find that each forms particles with different morphological characteristics. Lauric acid particles are large and irregular clusters, myristic acid particles are small and oval shaped, and palmitic acid particles form fibril-like particles and small circular clusters (Figure 2a-c). These unique morphological characteristics suggest the presence of free fatty acid particles that can then be confirmed with FMM using labeled fluorescence.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Aura PTx System and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2190"><strong>Aura+ System</strong></a> can easily detect the major degradation components of PS20 in proteincontaining samples at any stage of the drug manufacturing process. The method only requires 5 µL of sample, is specific and sensitive, and can analyze 96 samples in just a few hours, far outperforming other techniques. Aura PTx System and Aura+ System can also identify and differentiate the key degraded particulates from polysorbate formulation by their distinguishable shape, appearance, and specific labeling with BODIPY FL C16. The Aura polysorbate assay can detect FFAs at concentrations relative to lauric acid above 9.38 µM (&gt;2183 counts/mL) and quantitate above 18.75 µM (&gt;2976 counts/mL).</p>

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