CN114235981B - Method for identifying perilla leaf essential oil by combining gas phase-mass spectrum-sniffing instrument and gas chromatography-ion mobility spectrometry - Google Patents
Method for identifying perilla leaf essential oil by combining gas phase-mass spectrum-sniffing instrument and gas chromatography-ion mobility spectrometry Download PDFInfo
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- 235000004347 Perilla Nutrition 0.000 title claims abstract description 90
- 239000000341 volatile oil Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001871 ion mobility spectroscopy Methods 0.000 title claims abstract description 17
- 244000124853 Perilla frutescens Species 0.000 title description 4
- 241000229722 Perilla <angiosperm> Species 0.000 claims abstract description 89
- 239000000126 substance Substances 0.000 claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 238000004458 analytical method Methods 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 5
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- 239000012159 carrier gas Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 9
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- 238000011161 development Methods 0.000 abstract description 3
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- 150000002500 ions Chemical class 0.000 description 8
- NPNUFJAVOOONJE-ZIAGYGMSSA-N β-(E)-Caryophyllene Chemical group C1CC(C)=CCCC(=C)[C@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-ZIAGYGMSSA-N 0.000 description 6
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- NPNUFJAVOOONJE-UHFFFAOYSA-N beta-cariophyllene Natural products C1CC(C)=CCCC(=C)C2CC(C)(C)C21 NPNUFJAVOOONJE-UHFFFAOYSA-N 0.000 description 3
- NPNUFJAVOOONJE-UONOGXRCSA-N caryophyllene Natural products C1CC(C)=CCCC(=C)[C@@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-UONOGXRCSA-N 0.000 description 3
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- 241000207199 Citrus Species 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 description 2
- 235000020971 citrus fruits Nutrition 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
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- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
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- LVHLZMUFIYAEQB-UHFFFAOYSA-N perilla ketone Chemical compound CC(C)CCC(=O)C=1C=COC=1 LVHLZMUFIYAEQB-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
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- YHQGMYUVUMAZJR-UHFFFAOYSA-N α-terpinene Chemical compound CC(C)C1=CC=C(C)CC1 YHQGMYUVUMAZJR-UHFFFAOYSA-N 0.000 description 2
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- VOXZDWNPVJITMN-ZBRFXRBCSA-N 17β-estradiol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@H](CC4)O)[C@@H]4[C@@H]3CCC2=C1 VOXZDWNPVJITMN-ZBRFXRBCSA-N 0.000 description 1
- 239000001278 2-(5-ethenyl-5-methyloxolan-2-yl)propan-2-ol Substances 0.000 description 1
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- YDXQPTHHAPCTPP-UHFFFAOYSA-N 3-Octen-1-ol Natural products CCCCC=CCCO YDXQPTHHAPCTPP-UHFFFAOYSA-N 0.000 description 1
- 235000019743 Choline chloride Nutrition 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- BRHDDEIRQPDPMG-UHFFFAOYSA-N Linalyl oxide Chemical compound CC(C)(O)C1CCC(C)(C=C)O1 BRHDDEIRQPDPMG-UHFFFAOYSA-N 0.000 description 1
- WSTYNZDAOAEEKG-UHFFFAOYSA-N Mayol Natural products CC1=C(O)C(=O)C=C2C(CCC3(C4CC(C(CC4(CCC33C)C)=O)C)C)(C)C3=CC=C21 WSTYNZDAOAEEKG-UHFFFAOYSA-N 0.000 description 1
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- 244000269722 Thea sinensis Species 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 235000018927 edible plant Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
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- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JPTOCTSNXXKSSN-UHFFFAOYSA-N methylheptenone Chemical compound CCCC=CC(=O)CC JPTOCTSNXXKSSN-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000491 multivariate analysis Methods 0.000 description 1
- BTSIZIIPFNVMHF-UHFFFAOYSA-N nor-leaf alcohol Natural products CCC=CCO BTSIZIIPFNVMHF-UHFFFAOYSA-N 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 239000010664 perilla essential oil Substances 0.000 description 1
- 231100000374 pneumotoxicity Toxicity 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
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- 229930006978 terpinene Natural products 0.000 description 1
- 150000003507 terpinene derivatives Chemical class 0.000 description 1
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- 235000013311 vegetables Nutrition 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a method for identifying perilla leaf essential oil by combining a gas phase-mass spectrum-sniffing instrument and a gas phase chromatography-ion mobility spectrometry. The identification method of the invention comprises the following steps: firstly, preparing perilla leaf essential oil samples, detecting the perilla leaf essential oil samples by adopting a gas phase-mass spectrum-sniffing instrument, and determining aroma components and relative content and aroma branches in different perilla leaf essential oil samples; then detecting perilla leaf essential oil samples by adopting gas chromatography-ion mobility spectrometry to obtain GC-IMS fingerprint patterns of volatile aroma components in different perilla leaf essential oils; and combining the detection results of the first two steps, and performing the difference analysis of aroma components, aroma contents and aroma branches on different perilla leaf essential oils. The identification method can realize the identification and the differentiation of the perilla leaf essential oil extracted by different chemical extraction methods, and can also realize the identification and the differentiation of the perilla leaf essential oil extracted by different extraction methods, thereby providing scientific guidance for the development and the application of the perilla leaf.
Description
Technical Field
The invention relates to a method for identifying perilla leaf essential oil by combining a gas phase-mass spectrum-sniffing instrument (GC-MS-O) and a gas chromatography-ion mobility spectrometry (GC-IMS), belonging to the technical field of chemical analysis and detection.
Background
Perilla frutescens is used as a common medicinal and edible plant resource, has long cultivation and use history in China and is widely distributed in areas. The purple perilla can be divided into wild resources and cultivation resources according to the output types, and the cultivation resources can be divided into medicinal cultivation resources, edible cultivation resources, seed cultivation resources and the like according to different purposes. Its abundant and diverse resource applications, due to the diversity of perilla chemical types, the main chemical type distinction can be divided into "perilla" used in the calendar herbal (medicinal) as follows: the fragrance is fresh and sweet, the leaves are purple, and the chemical type of the tea is mainly n-amyl furan and perillaldehyde; perilla leaf as "Perilla frutescens" for cooking cooked food: the fragrance is lighter, the leaves are slightly sweet, the leaves are all green and wide round, and the main chemical type is beta-caryophyllene and 2-acyl furan chemical type; vegetable leaves are used as purple perilla for raw seafood auxiliary materials: the spicy fragrance has characteristic oil-green fragrance like perilla aldehyde, has faint scent of lemon, has full green leaves and small area, has obvious edge saw teeth, and has main chemical formula of the perilla aldehyde and the limonene; and other chemical forms such as the stachyone type and variants thereof. Studies have proved that perilla ketone type perilla leaves can cause lung toxicity after being eaten by livestock, so that the perilla resources can be applied and produced after analysis and identification of different perilla leaf chemical types are needed.
The existing method for identifying the chemical type of the perilla is mainly to extract essential oil in leaves of plants of the perilla, analyze and detect the components of the essential oil of the perilla, and the analysis and detection method of the chemical components of the essential oil is mainly gas phase-mass spectrometry (GC-MS), so that the method is mature, but the pretreatment is complex, and the difference comparison between samples is not easy.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the existing analysis and identification method of the perilla leaf essential oil has the problems of complex pretreatment, low sensitivity, low accuracy, low specificity and the like.
In order to solve the technical problems, the invention provides a method for identifying perilla leaf essential oil by combining a gas phase-mass spectrum-sniffing instrument and a gas phase chromatography-ion mobility spectrometry, which comprises the following steps:
step 1: preparing a perilla leaf essential oil sample;
step 2: detecting the perilla leaf essential oil samples prepared in the step 1 by adopting a gas phase-mass spectrum-sniffing instrument, and determining aroma components and relative content and aroma branches in different perilla leaf essential oil samples;
Step 3: detecting the perilla leaf essential oil sample prepared in the step 1 by adopting gas chromatography-ion mobility spectrometry to obtain GC-IMS fingerprint patterns of volatile aroma components in different perilla leaf essential oils;
Step 4: and (3) combining the results of the step (2) and the step (3), and performing the difference analysis of aroma components, aroma contents and aroma branches on different perilla leaf essential oils.
Preferably, the perilla leaf essential oil sample in the step 1 is perilla leaf essential oil extracted from perilla leaves of different chemical types or perilla leaf essential oil extracted by different extraction methods.
Preferably, in the step 2, a gas chromatography column model of 60m×0.25mm×0.25 μm is used for detection by a gas-mass spectrometer-sniffer; the conditions for detection by the gas chromatographic column are as follows:
sample injection amount: 0.2 μl;
split ratio: 10:1;
Carrier gas: helium gas;
flow rate: 2mL/min;
initial column temperature: maintaining at 50deg.C for 2min;
Heating program: heating to 115 ℃ at 8 ℃/min; heating to 200 ℃ at a speed of 2 ℃/min, and keeping for 3min; finally, the temperature reaches 230 ℃ at a rate of 4 ℃/min.
Preferably, in the gas phase-mass spectrum-sniffer detection, the detection conditions of the mass spectrum are:
Ionization mode: EI mode;
ionization energy: 70eV;
Ion source temperature: 230 ℃;
Scanning mode: a full scan mode;
Scanning range: m/z is 30-450;
Scanning rate: 1scan/s.
Preferably, the specific method for detecting by gas chromatography-ion mobility spectrometry in the step 3 is as follows: taking 200 mu L of perilla leaf essential oil sample in a sample bottle, and incubating for 15min at 80 ℃ and 500 r/min; then, carrying out headspace sample injection under the condition that the temperature of a sample injection port is 85 ℃; the column is kept at 60 ℃ under isothermal condition, and the carrier gas is nitrogen; eluting by adopting a program boosting mode, and detecting the gas separated by the gas chromatography capillary column in an ion migration tube; the carrier gas in the ion migration tube is nitrogen, the carrier gas flow is 150mL/min, and the detection temperature is 45 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the method for identifying the perilla leaf essential oil by combining the gas phase-mass spectrum-sniffing instrument (GC-MS-O) and the gas phase chromatography-ion mobility spectrometry (GC-IMS), the characteristics of GC-MS-O detection chemical components, aroma characteristics and intensity are combined with the characteristics of GC-IMS that the chemical components can be directly sampled and accurately detected through headspace, so that the chemical components and aroma analysis of the perilla leaf essential oil are detected more comprehensively and accurately, quantitative and qualitative analysis of the aroma components in the perilla leaf essential oil can be realized, and the perilla leaf essential oil from different sources can be accurately distinguished;
2. The identification method of the invention not only can realize the identification of the perilla leaf essential oil extracted by different chemical types, but also can identify and distinguish the perilla leaf essential oil extracted by different extraction methods, thereby providing scientific guidance for the development and application of the perilla leaf.
Drawings
FIG. 1 shows the leaves of Perilla frutescens of different chemical types;
FIG. 2 is a diagram of the shunt radar of the Perillae herba She Xiangqi of different chemical types;
FIG. 3 is a GC-IMS spectrum of the extracted perilla leaf essential oil (top view);
FIG. 4 is a graph showing the difference of the gas phase ion mobility spectrometry of the extracted perilla leaf essential oil;
FIG. 5 is a Gallery Plot of the extracted perilla leaf essential oil (fingerprint);
FIG. 6 is a principal component analysis chart of the extracted perilla leaf essential oil;
fig. 7 is a fingerprint similarity analysis (euclidean distance).
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1
Extracting the perilla leaf essential oil with different chemical formulas by adopting a water extraction method:
And mixing 20g of dry leaf powder of perilla leaves with different chemical types (shown in figure 1, wherein the left graph of A1 and A2 is the back surface of the leaf, the right graph is the front surface of the leaf, the front surface and the back surface of A1 are both green, and the front surface of A2 is purple and green), and then distilling with water vapor for 3h to obtain perilla leaf essential oil A1 and A2.
Example 2
Extracting perilla leaf essential oil with different chemical formulas by using deep eutectic solution:
20g of dry perilla leaf powder is mixed with 72g of natural deep eutectic solution (choline chloride: malic acid, molar ratio 2:1) and then mixed in 1000mL of distilled water. And distilling the mixed solution for 3h to obtain the perilla leaf essential oils B1 and B2. B1 and A1 use the same perilla leaf, and B2 and A2 use the same perilla leaf.
Example 3
GC-MS-O detects the chemical components of the perilla leaf essential oil:
GC-MS-O detection analysis was performed on the perilla leaf essential oils A1, A2, B1 and B2 obtained in example 1 and example 2, respectively. Detection conditions: the sample injection amount is 0.2 mu L, the split ratio is 10:1, the carrier gas is helium, and the flow rate is 2mL/min. The initial column temperature is 50 ℃, the temperature is kept for 2min, and the subsequent temperature rising procedure is as follows: heating to 115 ℃ at 8 ℃/min; heating to 200 ℃ at a speed of 2 ℃/min, and keeping for 3min; finally, the temperature reaches 230 ℃ at a rate of 4 ℃/min. The detection conditions of the mass spectrum are as follows: EI ionization mode, 70eV, ion source temperature 230 ℃, full scan mode, scan range of m/z30-450, scan rate of 1scan/s. The gas-mass spectrum analysis was performed while the fragrance was smelled (the sensory evaluator trained in the profession performed the smell, repeated the experiment three times, described the smell obtained, and recorded the fragrance intensity and time points thereof). The GC-MS-O analysis results are shown in tables 1-4 and FIG. 2.
TABLE 1 GC-MS-O analysis results of perilla leaf essential oil A1
TABLE 2 GC-MS-O analysis results of perilla leaf essential oil A2
TABLE 3 GC-MS-O analysis results of perilla leaf essential oil B1
TABLE 4 GC-MS-O analysis results of perilla leaf essential oil B1
Wherein the fragrance intensity is from 0-5 to weak to strong. As is clear from tables 1 to 4 and FIG. 2, the essential oils A1 and A2 of the different chemical type perilla leaves have different chemical compositions and fragrances. In the GC-MS-O result, the main component in A1 is l-perillaldehyde (relative content 64.29%), beta-caryophyllene (relative content 7.50%), linalool (relative content 1.49%); the main components in A2 are 2-acetyl furan (relative content 69.83%), cis-3-hexene-1-alcohol (relative content 4.42%) and beta-caryophyllene (relative content 4.11%). In terms of fragrance, xin Xiangjiang for A1 was stronger than A2, A2 had a citrus and grass green fragrance. The chemical components and the aroma of the perilla leaf essential oil subjected to NADES pretreatment are different. The main components in B1 and B2 are similar to the main components in A1 and A2 respectively: b1 is l-perillaldehyde (relative content 61.29%), and B2 is 2-acetyl furan (relative content 54.20%); b1 and B2 have stronger grass green fragrance, the spicy fragrance of B1 is stronger, and the citrus fragrance, the costustoot and the flower fragrance in B2 are stronger.
Example 4
GC-IMS detects the chemical components of the perilla leaf essential oil:
Respectively taking 200 mu L of perilla leaf essential oil A1, A2, B1 and B2 in a sample bottle, and incubating for 15min at 80 ℃ and 500 r/min; then, carrying out headspace sample injection under the condition that the temperature of a sample injection port is 85 ℃; the column is kept at 60 ℃ under isothermal condition, and the carrier gas is nitrogen; eluting by adopting a program boosting mode, and detecting the gas separated by the gas chromatography capillary column in an ion migration tube; the carrier gas in the ion migration tube is nitrogen, the carrier gas flow is 150mL/min, and the detection temperature is 45 ℃. The detection results are shown in FIGS. 3 to 6. In fig. 3 and 4, the vertical line at the abscissa 1.0 is the RIP peak (reactive ion peak, normalized). The ordinate represents the retention time(s) of the gas chromatograph, and the abscissa represents the ion migration time (normalization process). Each dot on either side of the RIP peak represents a volatile organic compound. Color represents the concentration of a substance, with darker color representing greater concentration. With respect to the difference plot, to more clearly compare differences between different samples, a difference contrast pattern may be employed: and selecting a spectrogram of one sample as a reference, and deducting the spectrogram of the other samples from the reference. If the volatile organics were identical, the subtracted background was white, while the dark color indicated the difference between the samples, and FIG. 4 is a graph of the difference made by selecting A1 as the reference.
As can be seen from the GC-IMS overall spectrum of fig. 3 and the difference graph of fig. 4, the perilla leaf essential oils A2 are similar to B2, and the A1, A2, A1, B1, A2, B2 have significant differences.
From the gallry Plot (fingerprint) of fig. 5, the differences in volatile substance types and concentrations of the 4 essential oils are evident. Combining the Principal Component Analysis (PCA) chart of FIG. 6 and the fingerprint similarity analysis chart of FIG. 7, it can be seen that the volatile substances of A2 and B2 are similar in the four samples, and the difference between the A1 and B1 essential oil samples is large. The concentration of the A1 sample is obviously higher than that of other samples, and the main substances which can be used as characteristic volatile substances for distinguishing the differences among the samples are as follows: linalool, Z-2-penten-1-ol, hexanol, terpinene, and the like. Similarly, the concentration of volatile substance species in the B1 sample was observed to be higher than that in the other samples, mainly from left to right: 2-methylbutyraldehyde, beta-myrcene, alpha-terpinene, 3-hydroxy-2-butanone, methyl heptenone, linalool oxide, 2-pentylfuran, and the like. The substances with the highest concentration in A2 are mainly: benzaldehyde, E-2, 4-heptenal, methyl acetate, 1-octen-3-ol, 4-methyl-2-one, E-2-valeraldehyde, Z-4-heptenal, E-3-hexene-1-aldehyde, and 3-octanone, and the like. The substances with the highest concentration in B2 are mainly: 1-penten-3-one, hexanal, and the like.
Consistent with the conclusion of the Gallery Plot, 4 samples can be distinguished by PCA and fingerprint similarity analysis, A2 is similar to B2, and A1 and B1, A2 and B2 and A1 and A2 have larger differences. Namely, the two types of perilla leaf essential oil with different chemical types are different, and the chemical components detected by the perilla leaf essential oil with the same chemical type obtained by different methods are also different.
In summary, the method for identifying perilla leaf essential oil by combining the gas phase-mass spectrum-sniffing instrument (GC-MS-O) and the gas phase chromatography-ion mobility spectrometry (GC-IMS) provides smelling aroma judgment on the basis of gas phase-mass spectrum combination by utilizing the gas phase-mass spectrum-sniffing instrument (GC-MS-O), thereby being beneficial to the component and aroma analysis of each chemical perilla leaf essential oil; meanwhile, the pretreatment by utilizing gas chromatography-ion mobility spectrometry (GC-IMS) is simple and convenient, the most original volatile chemical components and aroma are reserved, the characteristics of the perilla essential oil can be truly reflected, the minimum detection limit of the IMS can reach ppb or even ppt level, the perilla leaves with volatile active ingredients can be accurately detected, the three-dimensional spectrogram of the perilla leaves is collected, and the samples are further analyzed by utilizing multivariate data analysis, so that the differences among varieties are compared. The GC-MS-O and the GC-IMS are combined to analyze and identify the perilla leaf essential oil with different chemical types, so that compared with single GC-MS analysis, the analysis of chemical substances can be performed more accurately, the characteristic aroma description is provided for the perilla leaf essential oil with different chemical types, and scientific guidance is provided for the development and utilization of the perilla leaf.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to be limiting in any way and in nature, and it should be noted that several modifications and additions may be made to those skilled in the art without departing from the invention, which modifications and additions are also intended to be construed as within the scope of the invention.
Claims (3)
1. A method for identifying perilla leaf essential oil by combining a gas-mass spectrum-sniffing instrument and a gas chromatography-ion mobility spectrometry, which is characterized by comprising the following steps:
step 1: preparing a perilla leaf essential oil sample;
step 2: detecting the perilla leaf essential oil samples prepared in the step 1 by adopting a gas phase-mass spectrum-sniffing instrument, and determining aroma components and relative content and aroma branches in different perilla leaf essential oil samples;
Step 3: detecting the perilla leaf essential oil sample prepared in the step 1 by adopting gas chromatography-ion mobility spectrometry to obtain GC-IMS fingerprint patterns of volatile aroma components in different perilla leaf essential oils;
step 4: combining the results of the step 2 and the step 3, and performing the difference analysis of aroma components, aroma contents and aroma branches on different perilla leaf essential oils;
In the step 2, a gas chromatography column model of 60m multiplied by 0.25mm multiplied by 0.25 mu m is adopted for detection by a gas-mass spectrum-sniffing instrument, and an HP-Innowax chromatographic column is adopted for detection; the conditions for detection by the gas chromatographic column are as follows:
sample injection amount: 0.2 μl;
split ratio: 10:1;
Carrier gas: helium gas;
flow rate: 2mL/min;
initial column temperature: maintaining at 50deg.C for 2min;
Heating program: heating to 115 ℃ at 8 ℃/min; heating to 200 ℃ at a speed of 2 ℃/min, and keeping for 3min; finally, the temperature reaches 230 ℃ at the speed of 4 ℃/min;
The specific method for detecting by adopting the gas chromatography-ion mobility spectrometry in the step 3 is as follows: taking 200 mu L of perilla leaf essential oil sample in a sample bottle, and incubating for 15min at 80 ℃ and 500 r/min; then, carrying out headspace sample injection under the condition that the temperature of a sample injection port is 85 ℃; the column is kept at 60 ℃ under isothermal condition, and the carrier gas is nitrogen; eluting by adopting a program boosting mode, and detecting the gas separated by the gas chromatography capillary column in an ion migration tube; the carrier gas in the ion migration tube is nitrogen, the carrier gas flow is 150mL/min, and the detection temperature is 45 ℃.
2. The method for identifying perilla leaf essential oil by combining a gas-mass spectrometer-sniffing instrument and a gas chromatography-ion mobility spectrometry according to claim 1, wherein the perilla leaf essential oil sample in the step 1 is perilla leaf essential oil extracted from perilla leaves with different chemical formulas or perilla leaf essential oil extracted by different extraction methods.
3. The method for identifying perilla leaf essential oil by combining a gas-mass spectrum-sniffing instrument and a gas chromatography-ion mobility spectrometry according to claim 1, wherein in the detection of the gas-mass spectrum-sniffing instrument, the detection conditions of the mass spectrum are as follows:
Ionization mode: EI mode;
ionization energy: 70eV;
Ion source temperature: 230 ℃;
Scanning mode: a full scan mode;
Scanning range: m/z is 30-450;
Scanning rate: 1scan/s.
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