Mechanochemistry offers a green, solid-state pathway for designing nanomaterials, while chemical aging provides precise control under mild conditions. This study combines both methods to create nonstoichiometric bismuth oxide nanosheets with exceptional adsorption and photocatalytic performance toward persistent organic pollutants.Detailed structural and compositional analyses revealed that strain-induced defect formation during grinding followed by chemical delamination under aging leads to the formation of defect-rich Bi₂O₂.₃₃ nanosheets. This mechanochemical-aging synthesis provides new insight into two-dimensional metal oxide design and expands the potential for sustainable nanomaterial production.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104">Mechanochemical-Aging Synthesis of Bismuth Oxide Nanosheets for Photocatalysis</a></h4>Delaney J. Hennes, Luke T. Coward, Chase G. Thurman, Oksana Love*, and Pin Lyu*ACS Mater. Au 2025, XXXX, XXX, XXX-XXX<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsmaterialsau.5c00104">https://doi.org/10.1021/acsmaterialsau.5c00104</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.Mechanochemistry, old techniques with new perspectives, has been reawakening the passion for exploring solid-state approaches toward chemical transformations and materials synthesis in a green and sustainable manner, due to its intrinsic solvent-free and eco-friendly nature. <a href="javascript:void(0);">(1−8)</a> More importantly, the driving force of the mechanochemical process, mechanical force, has provided a fundamentally different reaction pathway by promoting intensive, well-oriented, and effective molecular collisions and creating molecular strains and structural defects, <a href="javascript:void(0);">(6,9−13)</a> compared to the conventional thermal or electrostatic driving forces. This perspective has opened new avenues for well-defined nanomaterial synthesis with unique structure–property relationships that the conventional solution-based methods cannot achieve, as well as in a greener way. <a href="javascript:void(0);">(4,14−17)</a> Recent reports have demonstrated great potential in designing metal and metal oxide nanoparticles, <a href="javascript:void(0);">(17,18)</a> nanocomposites, <a href="javascript:void(0);">(19)</a> and hybrid porous materials such as metal–organic frameworks (MOFs) and covalent organic frameworks (COFs) with desired properties. <a href="javascript:void(0);">(20−22)</a>In terms of 2D nanostructure design, two traditional approaches─bottom-up and top-down synthesis─have been widely developed in various synthesis strategies, offering precise control over size, shape, morphology, and dimensions. <a href="javascript:void(0);">(23,24)</a> The formation mechanism behind the scenes can be monitored and reasonably interpreted by advanced in situ spectroscopic <a href="javascript:void(0);">(25−27)</a> or microscopy methods, <a href="javascript:void(0);">(28−30)</a> to identify the critical factors in the structure transformation that lead to property-on-demand synthesis. Specifically, in 2D metal oxide nanosheet synthesis (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104#sch1">Scheme 1</a>), chemical vapor deposition, solvothermal method, and chemical exfoliation represent three typical methods. The first two methods start with molecular or atomic precursors for self-assembly growth, while the last method utilizes bulk layered host materials for layer-by-layer delamination. However, these methods rely on sophisticated instrumentation, harsh synthesis conditions, excess solvents, or toxic exfoliating chemicals, which limit their potential scalability.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Mater_Au_2025_Scheme_1_Comparison_of_Conventional_and_Mechanochemical_Aging_Methods_for_Bismuth_Oxide_Nanosheet_Synthesis_536967aa25.jpg" alt="ACS Mater. Au 2025: Scheme 1. Comparison of Conventional and Mechanochemical-Aging Methods for Bismuth Oxide Nanosheet Synthesis" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Mater_Au_2025_Scheme_1_Comparison_of_Conventional_and_Mechanochemical_Aging_Methods_for_Bismuth_Oxide_Nanosheet_Synthesis_536967aa25.jpg 245w," sizes="100vw" width="1000" height="487">Mechanochemical synthesis, with its all-solid-state, solvent-free nature, provides an alternative approach. This approach introduces an external applied physical force to initiate intense molecular interactions for mixing and growing (bottom-up) or to spread the shear stress or shock impact uniformly for deformation or delamination (top-down). It has been elegantly demonstrated in various traditional two-dimensional materials syntheses, such as graphene, <a href="javascript:void(0);">(31)</a> MXenes, <a href="javascript:void(0);">(32)</a> and transition-metal dichalcogenides. <a href="javascript:void(0);">(33)</a> Specifically, for bismuth-based materials, nanosheets of bismuthene, <a href="javascript:void(0);">(34)</a> bismuth oxyhalides, <a href="javascript:void(0);">(35)</a> and bismuth nitrates <a href="javascript:void(0);">(36)</a> have been reported previously with the mechanochemical methods. Meanwhile, very few reports are focused on metal oxide 2D nanostructures, probably due to the relatively higher interlayer interactions in those host materials. Thus, a follow-up process is needed to accelerate delamination of the mechanochemically produced bulk materials into the desired 2D nanosheet structure. Recently, Moores’s and Friščić’s groups have successfully demonstrated the combination of mechanochemistry and aging for the extraction and functionalization of biomass derivatives, <a href="javascript:void(0);">(37,38)</a> and functionalized inorganic metal or binary nanoparticle synthesis. <a href="javascript:void(0);">(39,40)</a> Aging, as a spontaneous diffusion-controlled process, can be controlled by the chemical reactivity and solution environment to induce material transformation, further advancing to the targeted structures while minimizing reagent and energy use. <a href="javascript:void(0);">(40)</a>In this work, we developed a mechanochemical-aging process to synthesize nonstoichiometric bismuth oxide (Bi2O2.33) nanosheets, which demonstrated excellent performance in the adsorption and photodegradation of perfluorooctanoic acid (PFOA). Through the observation of morphological, crystal structure, and surface chemistry changes during the aging process, we propose a strain-to-defect growing mechanism. Mechanical force exerted on metal precursors and reducing agents during solid-state grinding can induce rapid and intense molecular collisions, leading to the generation of strain-rich metallic nanostructures. The following aging process, occurring in an aqueous surfactant-deficient environment, can delaminate the bulk structure into well-defined 2D nanosheets over time with the assistance of ambient oxygen. This approach could potentially be applied to other 2D metal oxide nanostructures.<h4>Experimental Methods</h4><h5>Chemicals and Characterizations</h5>All chemicals and reagents were used without any purification. Bismuth(III) nitrate pentahydrate (99.999%, trace metal basis), PVP (M.W. 40,000), and sodium borohydride (99%, powder) were purchased from Thermo Scientific Chemicals. The morphology and elemental mapping analysis of bismuth oxide nanosheets (Bi2O2.33 nanosheets) was examined by scanning electron microscopy (SEM, JSM-IT700HR, 15 kV, JEOL) with energy dispersive X-ray spectroscopy (EDS, 0–20 kV energy window, Ultim Max 40: UVA13205 detector, Oxford Instruments). The evolution of the local crystalline structure of Bi2O2.33 nanosheets was monitored by a powder X-ray diffraction pattern (PXRD, Bruker D2 PHASER Benchtop XRD, Cu tubes, 30 kV, 10 mA) and was processed with DIFFRAC.EVA data analysis software with the Crystallography Open Database (rev.278581). The surface status of functional groups was determined by Fourier transform infrared spectroscopy (FTIR, Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=IRSpirit">IRSpirit</a>, 16 scans collected with a resolution of 4 cm–1) with the attenuated total reflectance (ATR) mode. The quantification of the PFOA (C7F15–COOH) and its degradation intermediates, perfluoroheptanoic acid (PFHpA, C6F13–COOH) and perfluorohexanoic acid (PFHxA, C5F11–COOH), was determined by liquid chromatography–mass spectrometry (LC-MS, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8040">LCMS-8040 Triple Quad LC-MS/MS</a>, Shimadzu Scientific Instruments) in negative electrospray ionization mode. Separation of analytes occurred with the use of a binary solvent gradient between 5 mM ammonium acetate in H2O and methanol that ramped from 5% methanol at 0–3 min to 40% methanol from 3 to 16 min and 80% methanol after 16 min. Each liquid was passed through a Phenomenex C18 column (1.8 μm, 100 × 2.1 mm) at a constant oven temperature of 40 °C with a solvent flow rate of 0.25 mL per min. The elution of PFOA occurred at 15.7 min, PFHpA at 13.2 min, and PFHxA at 11.6 min. A 13C isotope-labeled PFOA internal standard (Wellington Laboratories) was paired with a 12C native PFOA solution to quantify each sample’s concentration. The standard curve for PFOA quantification ranges from 0.5, 1, 5, 10, 25, 50, and 100 ppb, with a limit of detection of 3.6 ppb and a limit of quantification of 11.1 ppb.<h4>Results and Discussion</h4>To pinpoint the growing mechanism behind the mechanochemical-aging process, morphological, crystal structure, and surface chemistry changes are monitored by using SEM, XRD, and FTIR, respectively. First, after freshly grinding, the gray powder was sent for XRD testing, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104#fig2">Figure 2</a>a as Sample (Day 1). All of the observed diffraction peaks match well with the standard PDF card of metallic bismuth, indicating the successful reduction of molecular bismuth precursors. There is a small peak around 12 degrees, which matches one of the broad peaks of PVP powder (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsmaterialsau.5c00104/suppl_file/mg5c00104_si_001.pdf">Figure S1</a>), which is anticipated at this stage since the PVP used in the precursor mixture is 5 times the weight of the bismuth salts and has not been washed away. There is another small peak around 29° that matches nonstoichiometric bismuth oxide, which will be discussed below. According to the previous report, <a href="javascript:void(0);">(50)</a> the overall hexagonal crystal structure with a rhombohedral unit cell (as shown by the gray connections in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104#fig2">Figure 2</a>b) is commonly observed at ambient conditions for metallic bismuth. Two bilayers within the hexagonal structure are separated by relatively weak van der Waals-like interactions, which provide space and relatively low energy barriers for the following aging process. As follows, during the aging process, with the assistance of PVP surfactant solutions and dissolved ambient oxygen, the metallic Bi gradually oxidizes, and the crystal structure becomes more amorphous, as observed with 3 broad peaks of XRD patterns in Day 4’s and Day 7’s samples. The PVP peaks are not observed in these samples in the XRD, possibly due to the disruptions of the ordered structure in the powder form when they are dispersed in a low concentration solution (0.5 mM). Eventually, on Day 10, a fully oxidized sample is formed, with a crystal structure matching the nonstoichiometric Bi2O2.33 standard card, and no distinct peaks are observed for metallic Bi anymore. Additionally, <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsmaterialsau.5c00104/suppl_file/mg5c00104_si_001.pdf">Figure S2</a> compares standard patterns for bismuth subcarbonate and three distinct phases of stoichiometric bismuth oxide with those of the Day 10 sample. None of these reference patterns match the observed pattern of the Day 10 sample, ruling out the presence of these phase impurities in our material. This mixed-valent (Bi2+ and Bi3+) electron-rich structure of nonstoichiometric Bi2O2.33 was previously reported in research using traditional synthesis methods mentioned above, which demonstrated excellent properties, such as UV-emitting photoluminescence, supercapacitance, ferromagnetism, and photocatalysis. <a href="javascript:void(0);">(41,43,47)</a> To the best of our knowledge, there have been no reports on the mechanochemistry-driven synthesis of this unique structure. To be specific, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104#fig2">Figure 2</a>c, the overall tetragonal structure consists of a mixture of Bi2O3 and Bi2O2 layers within the lattice, possibly coming from the oxidation of metallic bismuth in the original bilayer structures before aging. This unique structure, featuring the stereochemically active lone pair of Bi3+ and the electrostatically electron-rich site of Bi2+, could potentially contribute to interlayer flexibility and defect formation, ultimately leading to the final nanosheet structure. This has been observed in other bismuth-based materials with preferred layered structures as well. <a href="javascript:void(0);">(51−53)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Mater_Au_2025_Figure_2_Structural_evolution_for_the_mechanochemical_aging_synthesis_process_a6c739235e.jpg" alt="ACS Mater. Au 2025: Figure 2. Structural evolution for the mechanochemical-aging synthesis process. (a) XRD spectra of samples collected on Day 1 (freshly made) and Days 4, 7, and 10 with the standard PDF reference cards for metallic Bi and nonstoichiometric Bi2O2.33. Schematic presentation of the crystal structures of (b) metallic Bi and (c) nonstoichiometric Bi2O2.33." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Mater_Au_2025_Figure_2_Structural_evolution_for_the_mechanochemical_aging_synthesis_process_a6c739235e.jpg 245w," sizes="100vw" width="2100" height="1168">Moving forward, the SEM images of freshly made (Day 1) samples and samples at different intervals during the aging process were collected for tracking morphological changes, along with EDS mapping to confirm the elemental composition and compare the spatial distribution of these elements. As shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmaterialsau.5c00104#fig3">Figure 3</a>, the bulk rod microstructure of metallic Bi after grinding and washing on Day 1 was observed with a relatively small amount of well-defined hexagonal thin nanosheets. These nanosheets have a relatively smooth surface, and the edge length is about 1 μm with a lateral width of 2 μm. The EDS full-range scan results also confirmed the dominant element compositions of carbon, oxygen, and bismuth in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsmaterialsau.5c00104/suppl_file/mg5c00104_si_001.pdf">Figure S3</a>, in which the carbon comes from both the carbon tape used in the sample preparation and the PVP polymer residues. For the EDS mapping in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsmaterialsau.5c00104/suppl_file/mg5c00104_si_001.pdf">Figure S4</a>, the distributions of Bi and O are relatively and consistently uniform across the sample, while the oxygen amount is significantly higher than the bismuth (estimated based on the spectra intensity counts and relative atomic mass). It is possible due to the residual PVP polymer still adsorbed on the surface, and is ready to participate in the next delamination process. This is also observed in the FTIR spectrum of O–H bending, C–H bending, and C–N stretching, possibly from the PVP, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsmaterialsau.5c00104/suppl_file/mg5c00104_si_001.pdf">Figure S5</a>, compared to the FTIR spectrum of PVP powder. It is noteworthy that very weak Bi–O bonding and a hydrophobic surface with almost no O–H stretching are also observed in Day 1’s sample, combined with the evidence of PVP, dominant metallic Bi peaks, and a small peak of Bi2O2.33 from the XRD analysis above. It is suggested that after freshly grinding, the metallic Bi bulk microrods formed as the aging precursor for the subsequent delamination process, and small amounts of oxide nanosheet structure began to form adjacent to the bulk rod, indicating a delamination pathway rather than nucleation from the aging solution.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Mater_Au_2025_Figure_3_Morphology_evolution_for_the_mechanochemical_aging_synthesis_process_9a69a3b684.jpg" alt="ACS Mater. Au 2025: Figure 3. Morphology evolution for the mechanochemical-aging synthesis process. SEM images of samples collected on (a–d) Day 1 (freshly made), (e–h) Day 4, (i–l) Day 7, and (m–p) Day 10." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Mater_Au_2025_Figure_3_Morphology_evolution_for_the_mechanochemical_aging_synthesis_process_9a69a3b684.jpg 205w," sizes="100vw" width="3000" height="2285"><h4>Conclusions</h4>In summary, we developed a mechanochemical-aging approach for the synthesis of nonstoichiometric Bi2O2.33 nanosheets, exhibiting excellent adsorption capacity and photocatalytic degradation performance toward forever chemicals. Different stages of morphological, crystal structure, and surface composition changes were observed and correlated to our proposed growth mechanism. Our mechanistic interpretation focuses on the effects of transient strain accumulation and relaxation resulting from applied mechanical forces during grinding, as well as controllable chemical delamination through capping ligands and oxygen amount during aging. This mechanism features strain-to-defect transformations at the molecular-to-crystal level, which could potentially extend to other 2D metal oxide nanostructure designs.

Mechanochemical-Aging Synthesis of Bismuth Oxide Nanosheets for Photocatalysis

This study presents a rapid and sensitive LC-MS/MS method for determining flibanserin in products marketed as female sexual desire enhancers. The method was fully validated according to ICH guidelines, achieving a low quantification limit and a short 5-minute analysis time. Confirmation was performed using LC-MS-IT-TOF.Analysis of commercial products revealed either the absence or only trace amounts of flibanserin, raising concerns about product authenticity, efficacy, and consumer safety. In addition, sustainability assessment demonstrated that the analytical approach is suitable for routine quality control applications.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004">Determination of Flibanserin in Female Sexual Desire Enhancer Products by LC–MS/MS and Its Confirmation by LCMS-IT-TOF</a></h4>Abeer Elriş, Mazlum Akif Altun, Saniye Özcan, Serkan Levent, and Nafiz Öncü Can*ACS Omega 2026, 11, 6, 10828–10836<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c13004">https://doi.org/10.1021/acsomega.5c13004</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.<div>In the world, many people experience sexual problems at some point in their lives. Women are disproportionately affected due to the lack of appropriate treatments in modern medicine, leading to most of them not receiving treatment or finding an appropriate solution. The research showed that one in every 10 women in the United States has some form of sexual dysfunction. <a href="javascript:void(0);">(1)</a> Flibanserin (FLB), an active substance that can be used especially in hypoactive sexual desire disorder (HSDD), has become a source of hope for many women with this problem.FLB was initially developed as an antidepressant; however, due to FLB’s inability to demonstrate an antidepressant effect in the experiments, participants indicated heightened sexual desire as a side effect, suggesting the potential application of this substance in the treatment of HSDD. So the Food and Drug Administration (FDA) approved FLB again in 2015, but this time for the treatment of HSDD instead of depression. <a href="javascript:void(0);">(2)</a> According to the data obtained from the begonia, daisy and violet studies, 12.8% of those taking FLB experienced side effects such as drowsiness, 10.6% dizziness, 9.9% nausea and 7.1% fatigue. <a href="javascript:void(0);">(3)</a> Due to these side effects, it is recommended that FLB be taken before going to bed. Also, taking FLB with alcohol was avoided due to the risk of fainting and hypotension.Although flibanserin (FLB) is one of the few active substances approved for the treatment of hypoactive sexual desire disorder, the number of available studies remains limited, as its approval by the FDA is relatively recent. The majority of published studies have focused on pharmaceutical quality control or bioanalytical applications, predominantly employing LC–MS/MS <a href="javascript:void(0);">(4−10)</a> and HPLC <a href="javascript:void(0);">(4,11)</a> techniques. These studies have investigated a wide range of sample matrices, including natural products such as beer, grape wine, and herbal tea, as well as biological samples (e.g., plasma and brain tissue) and pharmaceutical formulations such as Veroxeserin. In contrast, a study conducted in Poland reported the presence of FLB in certain herbal products, raising concerns regarding the unauthorized use of this compound. <a href="javascript:void(0);">(7)</a> This finding prompted questions about the potential presence of FLB in products marketed as female sexual desire enhancers in the Turkish market. Therefore, the present study aimed to determine FLB in various commercially available products obtained in Türkiye to assess the presence of FLB and to characterize their contents. Notably, it was observed that some products lacked manufacturer address information, despite regulatory requirements, and that the recommended usage instructions were concerning, particularly in light of the known side effects of FLB.This study aimed to develop and validate a sensitive and reliable LC–MS/MS method for the determination of flibanserin (FLB) in commercial products collected from the Turkish market that are marketed as female sexual desire enhancers. The samples were additionally analyzed using an LC-MS-IT-TOF instrument to support the qualitative characterization of their contents. A further objective of this work was to investigate whether FLB is being inappropriately incorporated into over-the-counter products in a manner analogous to the illicit use of sildenafil in food products or dietary supplements. By screening products predominantly obtained through online sales channels, this study sought to assess the potential unauthorized presence of FLB and to highlight possible risks to women’s health associated with such unregulated practices. As a complementary aspect, the environmental and practical performance of the proposed analytical approach was evaluated using greenness, whiteness, and blueness assessment tools, including ComplexMoGAPI, AGREE, WAC, and BAGI.<h4>2. Experimental Section</h4><h5>2.2. Instrumentation</h5>The mass spectrometric studies were succeeded in an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=8040">8040 model MS/MS</a> instrument connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+XR">Nexera XR Series LC</a> (from Shimadzu); the whole system was composed with DGU-20A3R degasser, LC-20AD gradient pump, SIL-20AC autosampler, CBM-20A communications bus module, CTO-10ASVP column oven.The LCMS-IT-TOF series liquid chromatography–high-resolution mass spectrometry instrument (Shimadzu) was used for structural characterization; the instrument consisted of the following modules: DGU-20A3 degasser, 2× LC-20AD gradient pump, SIL-20A autosampler, CTO-10ASVP column oven, CBM-20A communication module, and ion-trap and time-of-flight (IT-TOF) mass spectrometer. LCMS Solutions 3.80 software was used for setting instrumental parameters and spectrum integration.<h4>3. Result and Discussion</h4><h5>3.1. Ionization Characteristics of Flibanserin</h5>Although the LC–MS/MS system has some financial disadvantages, its ability to detect even very low concentrations makes it a suitable system for this study. Analyses were performed to determine the ionization type, and it was determined that FLB causes positive ionization. The daughter ions and collision energy observed under multiple reaction conditions using the electrospray ionization method are given in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#tbl2">Table 2</a>. The waiting time was determined to be 100 ms. Three daughter ions were detected, 161.05, 119.05, and 133.05 m/z. Their fragmentation paths are given in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#fig1">Figure 1</a>. It is suggested that the daughter ion with the m/z value of 161.05 is fragmented by heterolytic fragmentation, the daughter ion with the m/z value of 133.05 is fragmented by heterolytic fragmentation and carbonyl release, and the ion with the m/z value of 119.05 is fragmented by McLafferty rearrangement and hydroxyl release. The product ions at m/z 161 and m/z 119 have been reported in previous studies, while the ion at m/z 133 is considered a transitional step and is formed in lower abundance than the other two. <a href="javascript:void(0);">(4,6)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_6_10828_10836_Figure_1_Fragmentation_paths_of_FLB_in_positive_electrospray_ionization_mode_79d6842698.jpeg" alt="ACS Omega 2026, 11, 6, 10828–10836: Figure 1. Fragmentation paths of FLB in positive electrospray ionization mode." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_6_10828_10836_Figure_1_Fragmentation_paths_of_FLB_in_positive_electrospray_ionization_mode_79d6842698.jpeg 245w," sizes="100vw" width="1458" height="807"><h5>3.7. Comparison of the Method with Data in the Literature</h5>The analytical methods developed for FLB analysis in the literature were summarized in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#tbl5">Table 5</a>. The methods could be divided into two parts: quality control and bioanalytical purposes. It was obvious that all the instrumentation systems used for bioanalytical analyses presented so far were LC–MS/MS. The methods developed for quality control analyses were based on analysis with HPLC and LC–MS/MS. Apart from these, there are two other high-throughput methods that were developed for various purposes. However, these two methods have significant disadvantages, such as requiring experience and mastery for routine analyses. <a href="javascript:void(0);">(17,18)</a> Poplawska et al. were created to analyze both FLB and tadalafil at the same time in herbal products using an LC system along with PDA, MS, and a charged aerosol detector, just like the method that was developed. <a href="javascript:void(0);">(7)</a> They also characterized herbal preparations with LCMS-IT-TOF. Compared to their method, our method has advantages such as a working range that was approximately 100 times and LOQ was 0.5 times lower. Also, they characterized 9 compounds in herbal products with high-resolution mass spectrometry studies. Our method used high-resolution mass spectrometry to characterize all samples from 9 different market brands in detail. In addition, starting from sample collection to final analysis, the principles of less environmental harm and efficient and sustainable analytical method development were considered and evaluated with 4 different metric tools, which is another originality of the our article. Moreover, this study encourages other researchers to focus on such synthetic products and assess their impact on public health. In certain societies, these products hold a peculiar appeal: their sale remains hidden, yet their use is widespread. As a result, the table already presents a detailed comparison of all the methods developed so far. <a href="javascript:void(0);">(19)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_6_10828_10836_Table_5_Comparison_with_Previous_Studies_5e930ca443.webp" alt="ACS Omega 2026, 11, 6, 10828–10836 - Table 5. Comparison with Previous Studies.webp" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_6_10828_10836_Table_5_Comparison_with_Previous_Studies_5e930ca443.webp 122w," sizes="100vw" width="625" height="797"><h4>4. Conclusion</h4>Due to the lack of the drug treatment for hypoactive sexual desire disorder in women and the feeling of shame or hesitation stemming from cultural reasons. People in many countries do not think about or try to seek medical help for this issue. This situation not only complicates the diagnosis of such diseases but also exposes those affected to potential harm. Many women who cannot get medical help or access treatments like flibanserin and bremelanotide, which are available in only a few countries, often seek other options. In this case, products marketed as sexual desire enhancers for women are based on taking advantage of people’s helplessness. When marketing such products, the following is stated: “If you want to make a sweet surprise for your partner without him knowing, it will be enough to drop 7–8 drops into her drink and wait for half an hour.” Beyond the fact that such statements could lead women to take these products against their will, marketing them in this way encouraging people to use them and making it seem normal is also wrong.FLB was licensed by the United States Food and Drug Administration as the only medication for the treatment of female sexual interest/arousal disorder of any degree. <a href="javascript:void(0);">(11)</a> The current LC–MS/MS method is a novel, simple, and time-saving analytical method for the determination of FLB with a low quantification limit. The method was fully validated and used to determine FLB in samples that were bought as a solution to the treatment of female sexual desire enhancement. It has been shown that some of the products did not include content information. In addition, it has also been determined that the manufacturer’s address was present in some products while not others. As a result of the analysis, in some products had low concentration of FLB, which was not enough to make an effect. When the same samples were given to LCMS-IT-TOF to characterization, it was shown that the contents of the product did not match with that given in the lists on their boxes, and they included substances like caffeine, lactose, and citric acid, which have no effect on the disease., Finally, analyzing products like this in detail and identifying any substances that may threaten human health is an important point in terms of public health, especially considering that patients using such products do not have any other solution in Türkiye or in the other countries.In the present study, a comprehensive screening of 15 finished products was conducted, making it one of the most extensive surveys of commercially available formulations reported in the literature to date. Owing to the nanogram-per-milliliter-level LOQ achieved with the developed LC–MS/MS method, the method offers not only a highly sensitive approach for the analysis of finished products but also a potential alternative for plasma and urine analyses in future bioanalytical applications. Furthermore, the method is distinguished by its strong ecological profile, demonstrated through multiple green analytical chemistry assessment tools, underscoring its suitability as an environmentally conscious analytical approach. Although the proposed method demonstrated favorable greenness, whiteness, and blueness characteristics, further enhancements in environmental performance may be achieved in future studies through the implementation of miniaturized or low-flow LC systems and the integration of automated sample preparation, which could reduce energy consumption and improve overall sustainability.Overall, the analytical strategy presented herein provides a robust and versatile platform that can be effectively utilized across pharmaceutical quality control laboratories, food and dietary supplement testing facilities, and a wide range of academic research settings. This study therefore represents a valuable contribution to the field by combining comprehensive product surveillance with a highly sensitive, validated, and sustainability-oriented analytical methodology.</div>

Determination of Flibanserin in Female Sexual Desire Enhancer Products by LC–MS/MS and Its Confirmation by LCMS-IT-TOF

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