Význam tématu
Analýza složení vonných olejů je klíčová pro potravinářský, kosmetický i farmaceutický průmysl, jelikož kvalita a charakter vůně ovlivňuje senzorické vlastnosti výrobků.
Detailní chromatografická analýza umožňuje identifikovat jednotlivé vůně a nečistoty, což je nezbytné pro vývoj, kontrolu kvality i řešení problémů s off-flavors.
Cíle a přehled studie / článku
Cílem bylo demonstrovat využití GC/MS Off-Flavor Analyzer v kombinaci s GCMS-TQ8040 NX pro snadnou a spolehlivou analýzu vonných složek v neodérových aroma olejích.
Studie se zaměřila na porovnání standardní scan analýzy s metodami SIM a MRM, včetně testů na vzorcích Jasmine, Lavender, Rose a Citrus s cílem ověřit selektivitu a odolnost vůči kontaminantům.
Použitá metodika a instrumentace
Automatizované vzorkování a analýza:
- AOC-20s Plus jako autosampler
- AOC-20i Plus jako auto-injektor, objem injekce 1 µl, split 1:5
- GCMS-TQ8040 NX s tlakovým řízením (44,5 kPa), nosný plyn He
- Kolona InertCap 5MS/Sil (30 m × 0,32 mm, 0,5 µm), program teploty 50 °C (5 min) → +10 °C/min → 250 °C (10 min)
- Detekční režimy: scan (m/z 45–500 amu), SIM a MRM (event time 0,3 min)
- Předúprava: přímá injekce rozpuštěných vzorků, podpora headspace, SPME, MonoTrap
Hlavní výsledky a diskuse
Porovnání scan, SIM a MRM analýzy ukázalo:
- Scan analýza s knihovními vyhledáváními identifikovala i dosud neregistrované složky (např. benzylacetát v jazmínu).
- MRM poskytuje vyšší selektivitu a přesnost identifikace, odolává interferencím kontaminantů (příklady: n-dekanal a n-dodekanal v jazmínu).
- Simultánní scan-SIM/MRM umožňuje kvalifikaci i kvantifikaci vůní v jednom běhu.
- Test s příměsí minerálního oleje potvrdil, že MRM dokáže správně rozlišit cílové ionty i v silně znečištěném vzorku.
Přínosy a praktické využití metody
Metoda nabízí:
- Rychlé a spolehlivé nastavení analýzy díky databázi Off-Flavor Analyzer.
- Automatizované vytváření metod a kalibrací pro SIM i MRM režimy.
- Možnost aproximativní kvantifikace složek na základě registračních dat kalibračních křivek.
- Univerzální aplikaci pro různé vzorky – od kosmetiky přes potraviny až po farmaceutické produkty.
Budoucí trendy a možnosti využití
Očekávané směry rozvoje:
- Rozšíření a zpřesnění databáze vůní s návazností na sensory data.
- Integrace pokročilých technik mikroextrakce a on-line vzorkování.
- Nasazení AI-podpořených nástrojů pro predikci vůně a automatickou interpretaci profilů.
- IoT propojení analytických stanic pro centralizované sledování kvality ve výrobě v reálném čase.
Závěr
Komplexní použití GC/MS Off-Flavor Analyzer s GCMS-TQ8040 NX prokázalo vysokou účinnost a spolehlivost při analýze vonných olejů.
Simultánní scan-SIM/MRM analýza výrazně zrychluje proces a zvyšuje přesnost, zejména v přítomnosti kontaminantů.
Výsledný postup nabízí robustní řešení pro výzkum i rutinní QA/QC laboratoře v oboru analytické chemie.
Obsah byl automaticky vytvořen z originálního PDF dokumentu pomocí AI a může obsahovat nepřesnosti.
User Benefits
Application
News
GC-MS
GCMS-TQ™8040 NX
Analysis of Fragrance Components in Aroma Oils
Using GC/MS Off-Flavor Analyzer
E. Shimbo, Y. Nagao
Using GC/MS Off-Flavor Analyzer, components analysis can be easily performed even on non-odorous fragrances.
The fragrance of samples can be easily evaluated by the sensory information registered in the database of GC/MS Off-Flavor
Analyzer.
By using GC-MS/MS, more reliable identifications are possible even for samples containing contaminants.
GC/MS Off-Flavor Analyzer
Although GC/MS is widely used for odor analyses, it requires a
great deal of effort to determine the analysis conditions and to
perform post-analysis. GC/MS Off-Flavor Analyzer is a system
that allows the efficient analysis of the odor-causing substances.
Fig. 1 shows the analysis flow of the GC/MS Off-Flavor Analyzer.
The system is compatible with three types of liquid-phase
columns. It can also be used for analysis with pretreatment
techniques, such as MonoTrap, solid-phase microextraction, and
headspace sampling, and supports analyses using a sniffer.
Furthermore,
the
calibration
curve
information
can
be
registered after the analysis of the sample for correction, which
enables approximate quantifications of detected components.
Fig. 1 Analysis Flow with GC/MS Off-Flavor Analyzer
Introduction
Fragrances are known to have various effects such as promoting
relaxation, masking unpleasant odors, and increasing appetite.
Therefore, the importance of fragrance is emphasized in many
fields, including daily necessities, cosmetics, and foods. While
sensory analyses by professionals are often used to evaluate
fragrances, analyses with gas chromatography enable detailed
components analyses of complex fragrances.
GC/MS Off-Flavor Analyzer is a database of expert information
for odor analyses. It is also known that odor-causing substances
produce
pleasant
smells
as
well,
depending
on
their
concentrations and compositions. In this article, we applied
GC/MS Off-Flavor Analyzer to the analyses of non-odorous
fragrances. Belows are the examples of how we used GCMS-
TQ8040 NX gas chromatograph mass spectrometer to investigate
the characteristics of aroma oil fragrances.
Table 1 Instrument Configuration and Analysis Conditions
Auto sampler
: AOC™-20s Plus
[AOC]
Auto injector
: AOC-20i Plus
Injection volume
: 1 μl
Instrument
: GCMS-TQ8040 NX
[GCMS]
Flow control mode
: Pressure (44.5 kPa)
Column temp. program
: 50 ˚C (5 min)
o 10 ˚C/min o 250 ˚C (10 min)
Injection mode
: Split (1 : 5)
Interface temp.
: 250 ˚C
Carrier gas
: He
Ion source temp.
: 200 ˚C
Purge flow rate
: 3 mL/min
m/z range
: 45-500 amu
Column
: InertCap 5MS/Sil
Event time
: 0.1 min (scan)
(30 m × 0.32 mm I.D., 0.5 μm)
0.3 min (SIM/MRM)
①Column and pretreatment device settings
②Standard sample analyses
④Automated method creation
⑤Target analyses/post analyses
· Standard sample for retention time correction (n-alkanes)
· Sample for instrument performance check
· Sample for calibration curve correction
③Retention time modifications by ARRT
Application
News
Analysis Conditions
Table 1 shows the instrument configuration and analysis
conditions used. Note that GC/MS Off-Flavor Analyzer supports
both SIM and MRM analyses. We performed simultaneous scan-
SIM and scan-MRM analyses using the analysis conditions
registered in GC/MS Off-Flavor Analyzer. Here we adopted a
simple test by directly injecting liquid samples.
The notes in the graphs show the "odor quality" of each
components. As shown in Fig.3, the fragrance characteristics of
detected components can be easily confirmed by the "odor
qualities" registered in the database of GC/MS Off-Flavor
Analyzer. For example, the components detected in Jasmine
had fragrances suggestive of plants. It is also found that
Lavender had many refreshing fragrances such as mint,
camphor, and anise, while Citrus, as its name suggested,
contained a high level of citrus fragrance.
Fig. 2 Ratios of Major Components and Flavor Characteristics of Four Aroma Oils
Vertical axis: ratio based on the value of the largest component in each analysis
Analysis of Aroma Oils
Four commercially available aroma oils (Jasmine, Lavender, Rose,
and Citrus) were diluted to 0.1 % with ethanol and then analyzed.
The graphs in Fig. 2 shows the ratios of major components and
fragrance characteristics obtained by SIM and MRM analyses.
The vertical axes refer the ratios based on the value of the
largest component in each analysis.
These graphs show major 8 components quantified by MRM
analysis, excluding those detected only by SIM analysis.
Major odor components
Sensory information
Fig. 3 A Part of Database in GC/MS Off-Flavor Analyzer
0
0.5
1
Sweet,
Flower
Geranium,
Rose
Flower,
Lavender
Honey, Spice,
Rose, Lilac
Jasmine
SIM
MRM
Sweet,
Mint
Flower,
Lavender
Camphor
Mint,
Anise, Oil
Lavender
SIM
MRM
Mint,
Citrus
Geranium,
Rose
Honey,
Clove
Citrus
SIM
MRM
0
0.5
1
Violet,
Wood
Rose
SIM
MRM
Honey, Spice,
Rose, Lilac
Application
News
Using the automated method creation tool of the GC/MS Off-
Flavor Analyzer, users can easily configure SIM and MRM
analysis conditions. Furthermore, scan analysis and SIM or MRM
analysis can be performed at the same time. Fig. 4 shows the TIC
chromatograms of four aroma oil samples obtained by
simultaneous scan-MRM analyses. With a chromatogram from
scan analysis, the peaks can be identified based on a widely-
used mass spectral library search. For example, the distinctive
peak (arrow in Fig. 4) in the chromatogram of Jasmine was
identified as benzyl acetate through the library search. Benzyl
acetate is a major ingredient of essential oils of flowers such as
jasmine, exhibiting a sweet scent. As in this example,
simultaneous scan-SIM/MRM analysis allows us to identify even
the components not registered in the database of GC/MS Off-
Flavor Analyzer.
Accurate Identifications by MRM Analysis
Fragrances are diversified by the combination of many
components. Furthermore, perfumes often contain nature-
derived ingredients such as plants, which contain a lot of
contaminants. These facts make it difficult to analyze the
composition of fragrances. For analysis of such samples, MRM
analysis is more suitable than SIM analysis because of its higher
selectivity. Below shows comparisons between SIM and MRM
analyses.
N-decanal in Jasmine sample (Fig. 5) was not identified in SIM
analysis due to the mismatch of the ion intensity ratio, but was
identified in MRM analysis. In addition, n-dodecanal (Fig. 6) was
identified in SIM analysis because the ion intensity ratio was
within the acceptable range, but not identified in MRM analysis.
In SIM analysis, contaminants can affect the peaks of the target
ions, preventing accurate identification. In the two examples
above, it is assumed that MRM analysis, the two steps of
fragmentation enabled more accurate identification.
Fig. 5 Chromatograms of n-decanal in Jasmine Sample
Jasmine
Citrus
Lavender
Rose
(min)
5.0
10.0
15.0
20.0
25.0
30.0
Fig. 4 TIC Chromatograms Obtained by Scan Analyses of Four Aroma Oil Samples (0.1 %)
(min)
13.2
13.4
13.6
13.8
14.0
0.0
%
100.0
128.00
112.00
57.0
intensi
ty
SIM
112.00>83.00
112.00>55.00
112.00>70.00
(min)
13.2
13.4
13.6
13.8
14.0
0.0
%
100.0
intensi
ty
MRM
82.00
96.00
57.00
(min)
16.4
16.6
16.8
17.0
17.2
0.0
%
100.0
intensi
ty
intensi
ty
110.00>81.00
140.00>70.00
110.00>67.00
(min)
16.4
16.6
16.8
17.0
17.2
0.0
%
100.0
SIM
MRM
Fig. 6 Chromatograms of n-dodecanal in Jasmine Sample
Application
News
www.shimadzu.com/an/
Shimadzu Corporation
Analytical & Measuring Instruments Division
Global Application Development Center
© Shimadzu Corporation, 2021
For Research Use Only. Not for use in diagnostic procedure.
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First Edition: Jun. 2021
01-00154-EN
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MonoTrap and InertCap are trademarks of GL Sciences, Inc. .
Fig. 7 Chromatograms of α-terpineol in Jasmine Sample
Conclusion
Commercially available aroma oils were analyzed with GCMS-
TQ8040 NX gas chromatograph mass spectrometer (Fig. 8).
Using GC/MS Off-Flavor Analyzer, we could easily confirm the
fragrance
characteristics
of
four
different
aroma
oils.
Simultaneous scan and SIM/MRM analysis enabled qualification
of components not registered in the database of GC/MS Off-
Flavor Analyzer.
Furthermore, although compositional analysis of perfumes such
as aroma oils is sometimes difficult due to the nature-derived
contaminants, the use of MRM analysis provided highly reliable
identifications of components. It resulted in more accurate
evaluation of the fragrances even with complex components.
We next analyzed Jasmine sample intentionally contaminated
with a small amount of mineral oil, imitating a nature-derived
sample with contaminants. Fig. 7 shows the chromatograms. In
the SIM analysis, the presence of mineral oil affected the ion
peak of α-terpineol. MRM analysis, however, enabled correct
identification even in the sample spiked with mineral oil.
(min)
13.2
13.4
13.6
13.8
0.0
%
100.0
43.00
59.00
136.00
intensi
ty
43.00
59.00
136.00
(min)
13.2
13.4
13.6
13.8
0.0
%
100.0
intensi
ty
136.00>93.00
121.00>93.00
136.00>121.00
(min)
13.2
13.4
13.6
13.8
0.0
%
100.0
intensi
ty
Sample blank
Spiked with
mineral oil
Spiked with
mineral oil
SIM
MRM
Fig. 8 GCMS-TQ™8040 NX + AOC™-20i+s
