CN109212102B - Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint - Google Patents
Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint Download PDFInfo
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Abstract
The invention discloses a method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint, which starts from volatile components of gardenia oil, analyzes and detects the volatile characteristic components of gardenia and gardenia oil by using headspace solid phase microextraction and combining a gas chromatography-mass spectrum combined technology, establishes a gas chromatography-mass spectrum characteristic fingerprint of the volatile components of the gardenia and the gardenia oil, and compares effective peaks of the characteristic fingerprint through evaluation software so as to identify the gardenia oil. The method has the advantages of complete retention of characteristic components of the characteristic fingerprint, high identification accuracy, strong anti-interference, simple operation and the like, and is a detection method capable of quickly identifying the gardenia oil.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrometry fingerprint.
Background
The gardenia is a small evergreen shrub belonging to the gardenia genus of the Rubiaceae family, is widely distributed in China, fruits of the gardenia are traditional Chinese medicines, belongs to the first batch of medical and edible dual-purpose resources issued by the ministry of health, and researches in recent years find that the oil content of the gardenia is close to that of soybeans, and the fatty acids of the gardenia mainly comprise linoleic acid, oleic acid and palmitic acid which respectively reach 50 percent, 20 percent and 20 percent, so that the gardenia is a functional oil material with rich nutrition, has the peculiar smell of the gardenia, has the effects of calming, hypnosis, anticonvulsion and promoting learning and memory, and can be used as a detection method for identifying the truth of the gardenia oil by establishing a gas chromatography-mass spectrometry fingerprint of characteristic components of the gardenia and the gardenia oil by utilizing the characteristic smell of the gardenia and the gardenia oil.
At present, the identification of edible oil mainly comprises the following three methods: (1) the variety of the oil or fat was determined by producing fatty acid methyl esters by transesterification and measuring the content of each fatty acid by gas chromatography. The main components of the gardenia oil are linoleic acid, oleic acid and palmitic acid which are similar to the main components of various other edible vegetable oils, so the characteristic components of the gardenia oil cannot be found out by the fatty acid methyl ester method, the truth and the falseness of the gardenia oil cannot be identified, and the conformity of the grease can be judged only through the content difference of each fatty acid. The pretreatment of the method is complex, and the used reagent has high toxicity. (2) Volatile components of the edible oil are extracted by a distillation method, and the volatile components are qualitatively analyzed by gas chromatography separation, so that the type of the edible oil is identified by the volatile component composition. However, the distillation method is long in time, and the distillation may cause structural changes of some volatile substances due to high temperature damage, and the gas chromatography cannot directly perform qualitative analysis on the components, so that the method cannot be used for identifying the authenticity of the gardenia oil. (3) The volatile components of the edible oil are measured to form a fingerprint, and the edible oil is identified through the fingerprint. However, the conventional fingerprint spectrum method only measures the volatile components of the edible oil to form a fingerprint spectrum, and does not measure the volatile components of the raw materials to form a common fingerprint spectrum. Because the content of some characteristic volatile components in the oil is greatly reduced after the raw materials are processed into the edible oil, although peaks still exist on a spectrogram, the peaks are possibly ignored when a fingerprint is formed due to the small peak area, and the components are just important characteristics of the edible oil. Therefore, the fingerprint spectrum is formed only by utilizing the volatile components of the edible oil, and the accurate identification of the edible oil cannot be realized. At present, no reliable method for identifying gardenia oil based on volatile component fingerprint spectrum is reported.
Disclosure of Invention
The invention mainly aims to solve the problem of difficult identification of the gardenia oil, develop a novel method for analyzing and detecting the volatile characteristic components of the gardenia oil based on headspace solid-phase microextraction and gas chromatography-mass spectrometry combined technology, and provide a convenient and reliable detection method for identifying the gardenia oil based on the gas chromatography-mass spectrometry fingerprint spectrum of the volatile characteristic components of the gardenia oil established by the established analysis method.
In order to achieve the purpose, the invention adopts the following technical means:
the method starts from the volatile components of the gardenia oil, analyzes and detects the volatile characteristic components of the gardenia and the gardenia oil by using headspace solid-phase microextraction and combining a gas chromatography-mass spectrometry combined technology, establishes a gas chromatography-mass spectrometry characteristic fingerprint spectrum of the volatile components of the gardenia and the gardenia oil, and compares effective peaks of the characteristic fingerprint spectrum by evaluation software, thereby realizing the identification of the gardenia oil. The method has the advantages of complete retention of characteristic components of the characteristic fingerprint, high identification accuracy, strong anti-interference, simple operation and the like, and is a detection method capable of quickly identifying the gardenia oil.
The method specifically comprises the following steps:
and (1) performing gas chromatography-mass spectrometry analysis on volatile components of the gardenia and the authentic gardenia oil. The method comprises the following specific steps: placing 1g fructus Gardeniae (pulverized by pulverizer after drying at 70 deg.C) or 1mL fructus Gardeniae oil in 20mL headspace sample injection bottle, rapidly sealing, inserting 50/30 μm DVB/CAR/PDMS extraction fiber, adsorbing volatile components at 60 deg.C for 40min, pulling out the extraction fiber, and rapidly inserting into gas chromatograph sample inlet for desorption for 5 min. The volatile components are separated and qualitatively analyzed by adopting a gas chromatography-mass spectrometer under the following chromatographic and mass spectrum conditions, each peak in a total ion flow diagram is searched and checked by a mass spectrum computer data system, a NIST14 LIBRARY standard mass spectrogram is searched and checked, and a compound with the matching degree of more than 85 percent can be used as an identification result to obtain a gas chromatography-mass spectrum spectrogram of the volatile components of the gardenia and the authentic gardenia oil (see figure 1).
Gas chromatography conditions: chromatography column, DB-5MS (30 m × 0.25mm × 0.25 μm) capillary column; temperature programming: maintaining at 40 deg.C for 4min, heating to 70 deg.C at 6 deg.C/min, maintaining for 8 min, heating to 180 deg.C at 6 deg.C/min, and maintaining for 3 min; the temperature of a sample inlet is 250 ℃; carrier gas He with the flow rate of 1 mL/min; no split stream, solvent delay 4 min.
Mass spectrum conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200 deg.C, interface temperature 250 deg.C.
And (2) establishing a characteristic fingerprint of the volatile component gas chromatography-mass spectrometry of the gardenia oil. According to the gas chromatography-mass spectrometry analysis result of volatile components of the gardenia and the authentic gardenia oil in the step (1), 11 common characteristic peaks of the gardenia and the gardenia oil are selected, wherein (1) the peak time is 5.631 minutes, Hexanal (Hexanal) and the mass-to-charge ratios are 56.05 and 72.10; (2) peak time 8.506 minutes, 1,3,5, 7-cyclooceteteraene (Cyclooctatetraene), mass to charge ratios 51.05, 78.05 and 104.10; (3) peak time 12.290 minutes, Furan, 2-pentyl- (2-n-pentylfuran), mass to charge ratios 53.05, 81.05 and 138.15; (4) the peak-out time is 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one (2, 2,5, 5-Tetramethyl-3-cyclopenten-1-one), the mass-to-charge ratio is 70.05, 95.10 and 110.15; (5) peak time 14.071 minutes, Benzene, 1,2, 3-trimethy- (1, 2, 3-trimethylbenzene), mass to charge ratios 104.10 and 120.15; (6) peak time 21.266 minutes, Isophorone (Isophorone), mass to charge ratios 54.05, 82.10 and 138.15; (7) peak time 22.239 minutes, 2,6, 6-trimethy-2-cyclohexene-1, 4-dione (4-oxoisoflurone), mass to charge ratios 68.00, 96.05 and 152.10; (8) peak time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6, 6-trimethy- (safinaldehyde), mass to charge ratios 91.10, 107.10, 121.15 and 150.15; (9) peak time 25.048 minutes, 4-Methyleneisopherone 4- (Methyleneisophorone), mass to charge ratios 91.05, 107.10 and 150.15; (10) peak time 27.662 minutes, nonaic acid (Nonanoic acid), mass to charge ratios 60.00, 73.05 and 115.10; (11) peak time 30.408 minutes, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol (2, 4,7, 9-Tetramethyl-5-decyne-4, 7-diol), mass to charge ratios 109.10 and 151.15. Characteristic fingerprint as gas chromatography-mass spectrometry of gardenia oil (see fig. 2).
And (3) identifying the gardenia oil. Taking a gas chromatography-mass spectrogram of volatile components of the commercial gardenia oil or unknown edible vegetable oil according to the step (1), comparing a characteristic fingerprint (figure 2) of the gas chromatography-mass spectrogram of the gardenia oil with a gas chromatography-mass spectrogram of the volatile components of the commercial gardenia oil or unknown edible vegetable oil by using a traditional Chinese medicine chromatography fingerprint similarity evaluation system, confirming common characteristic peaks of 11 gardenia and gardenia oil, and distinguishing effective peaks according to the condition that the retention time difference is less than 0.1min, the mass-to-charge ratio difference is less than 0.05 and the relative peak area is more than 0.5%, wherein 9 common characteristic peaks appear and are confirmed to be the gardenia oil and less than 9 common characteristic peaks appear and are confirmed to be the non-gardenia oil.
The invention has the beneficial effects that:
(1) the method is used for identifying the truth of the gardenia oil, and the characteristic volatile components in the gardenia oil are completely analyzed by using gas chromatography-mass spectrometry to form a fingerprint, so that the identification accuracy and reliability are improved, and the defect of abstract sensory analysis is overcome.
(2) The fingerprint contains 11 common characteristic peaks of gardenia and gardenia oil, the accuracy and reliability are high, the applicability is wide, the speed is high, the cost is low, the established method can quickly identify the gardenia oil, the identification time is less than 90 minutes, the accuracy rate can reach 100%, each sample identification consumable is only a headspace bottle cap, and the cost is lower than 10 yuan.
(3) The fingerprint data made from common characteristic peaks of volatile components of the gardenia and the gardenia oil can be stored in working software for long-term use without correction.
Drawings
FIG. 1 shows the gas chromatography-mass spectrometry analysis of volatile components of Gardenia jasminoides ellis (a) and Gardenia oil (b) according to the present invention;
FIG. 2 is a gas chromatography-mass spectrometry characteristic fingerprint spectrum of an embodiment of the present invention including 11 common characteristic peaks of gardenia and gardenia oil, used as gardenia oil;
FIG. 3 is a comparison of the volatile component gas chromatography-mass spectrometry profile of a commercially available gardenia oil and the gas chromatography-mass spectrometry signature fingerprint of the gardenia oil;
FIG. 4 is a comparison of the volatile component gas chromatography-mass spectrometry profile of other commercially available vegetable oils and the gas chromatography-mass spectrometry signature of gardenia oil.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
The identification of the gardenia oil sold in the market specifically comprises the following steps:
and (1) performing gas chromatography-mass spectrometry analysis on volatile components of the gardenia and the authentic gardenia oil. The method comprises the following specific steps: placing 1g fructus Gardeniae (pulverized by pulverizer after drying at 70 deg.C) or 1mL fructus Gardeniae oil in 20mL headspace sample injection bottle, rapidly sealing, inserting 50/30 μm DVB/CAR/PDMS extraction fiber, adsorbing volatile components at 60 deg.C for 40min, pulling out the extraction fiber, and rapidly inserting into gas chromatograph sample inlet for desorption for 5 min. The volatile components are separated and qualitatively analyzed by adopting a gas chromatography-mass spectrometer under the following chromatographic and mass spectrum conditions, each peak in a total ion flow diagram is searched and checked by a mass spectrum computer data system, a NIST14 LIBRARY standard mass spectrogram is searched and checked, and a compound with the matching degree of more than 85 percent can be used as an identification result to obtain a gas chromatography-mass spectrum spectrogram of the volatile components of the gardenia and the authentic gardenia oil (see figure 1).
Gas chromatography conditions: chromatography column, DB-5MS (30 m × 0.25mm × 0.25 μm) capillary column; temperature programming: maintaining at 40 deg.C for 4min, heating to 70 deg.C at 6 deg.C/min, maintaining for 8 min, heating to 180 deg.C at 6 deg.C/min, and maintaining for 3 min; the temperature of a sample inlet is 250 ℃; carrier gas He with the flow rate of 1 mL/min; no split stream, solvent delay 4 min.
Mass spectrum conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200 deg.C, interface temperature 250 deg.C.
And (2) establishing a characteristic fingerprint of the volatile component gas chromatography-mass spectrometry of the gardenia oil. According to the gas chromatography-mass spectrometry analysis result of volatile components of the gardenia and the authentic gardenia oil in the step (1), 11 common characteristic peaks of the gardenia and the gardenia oil are selected, wherein (1) the peak time is 5.631 minutes, Hexanal (Hexanal) and the mass-to-charge ratios are 56.05 and 72.10; (2) peak time 8.506 minutes, 1,3,5, 7-cyclooceteteraene (Cyclooctatetraene), mass to charge ratios 51.05, 78.05 and 104.10; (3) peak time 12.290 minutes, Furan, 2-pentyl- (2-n-pentylfuran), mass to charge ratios 53.05, 81.05 and 138.15; (4) the peak-out time is 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one (2, 2,5, 5-Tetramethyl-3-cyclopenten-1-one), the mass-to-charge ratio is 70.05, 95.10 and 110.15; (5) peak time 14.071 minutes, Benzene, 1,2, 3-trimethy- (1, 2, 3-trimethylbenzene), mass to charge ratios 104.10 and 120.15; (6) peak time 21.266 minutes, Isophorone (Isophorone), mass to charge ratios 54.05, 82.10 and 138.15; (7) peak time 22.239 minutes, 2,6, 6-trimethy-2-cyclohexene-1, 4-dione (4-oxoisoflurone), mass to charge ratios 68.00, 96.05 and 152.10; (8) peak time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6, 6-trimethy- (safinaldehyde), mass to charge ratios 91.10, 107.10, 121.15 and 150.15; (9) peak time 25.048 minutes, 4-Methyleneisopherone 4- (Methyleneisophorone), mass to charge ratios 91.05, 107.10 and 150.15; (10) peak time 27.662 minutes, nonaic acid (Nonanoic acid), mass to charge ratios 60.00, 73.05 and 115.10; (11) peak time 30.408 minutes, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol (2, 4,7, 9-Tetramethyl-5-decyne-4, 7-diol), mass to charge ratios 109.10 and 151.15. Characteristic fingerprint as gas chromatography-mass spectrometry of gardenia oil (see fig. 2).
Step (3) identification: taking a gas chromatography-mass spectrogram of volatile components of the commercially available gardenia oil according to the step (1), comparing the characteristic fingerprint (figure 2) of the gas chromatography-mass spectrogram of the gardenia oil with the gas chromatography-mass spectrogram of the volatile components of the commercially available gardenia oil by utilizing a traditional Chinese medicine chromatography fingerprint similarity evaluation system, confirming common characteristic peaks of 11 gardenia oils and the gardenia oils, and distinguishing the effective peaks according to the condition that the retention time difference is less than 0.1min, the mass-to-charge ratio difference is less than 0.05 and the relative peak area is more than 0.5 percent, wherein 9 of the effective peaks are confirmed to be gardenia oil and less than 9 of the effective peaks are confirmed to be non-gardenia oil.
FIG. 3 is a comparison of the gas chromatography mass spectrum of the volatile component of the commercially available gardenia oil and the characteristic fingerprint spectrum of the gas chromatography-mass spectrum of the gardenia oil, and shows that 11 common characteristic peaks can be found in the gas chromatography-mass spectrum of the volatile component of the commercially available gardenia oil (see FIG. 3).
Example 2
The identification of other commercially available vegetable oils specifically comprises the following steps:
and (1) performing gas chromatography-mass spectrometry analysis on volatile components of the gardenia and the authentic gardenia oil. The method comprises the following specific steps: placing 1g fructus Gardeniae (pulverized by pulverizer after drying at 70 deg.C) or 1mL fructus Gardeniae oil in 20mL headspace sample injection bottle, rapidly sealing, inserting 50/30 μm DVB/CAR/PDMS extraction fiber, adsorbing volatile components at 60 deg.C for 40min, pulling out the extraction fiber, and rapidly inserting into gas chromatograph sample inlet for desorption for 5 min. The volatile components are separated and qualitatively analyzed by adopting a gas chromatography-mass spectrometer under the following chromatographic and mass spectrum conditions, each peak in a total ion flow diagram is searched and checked by a mass spectrum computer data system, a NIST14 LIBRARY standard mass spectrogram is searched and checked, and a compound with the matching degree of more than 85 percent can be used as an identification result to obtain a gas chromatography-mass spectrum spectrogram of the volatile components of the gardenia and the authentic gardenia oil (see figure 1).
Gas chromatography conditions: chromatography column, DB-5MS (30 m × 0.25mm × 0.25 μm) capillary column; temperature programming: maintaining at 40 deg.C for 4min, heating to 70 deg.C at 6 deg.C/min, maintaining for 8 min, heating to 180 deg.C at 6 deg.C/min, and maintaining for 3 min; the temperature of a sample inlet is 250 ℃; carrier gas He with the flow rate of 1 mL/min; no split stream, solvent delay 4 min.
Mass spectrum conditions: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200 deg.C, interface temperature 250 deg.C.
And (2) establishing a characteristic fingerprint of the volatile component gas chromatography-mass spectrometry of the gardenia oil. According to the gas chromatography-mass spectrometry analysis result of volatile components of the gardenia and the authentic gardenia oil in the step (1), 11 common characteristic peaks of the gardenia and the gardenia oil are selected, wherein (1) the peak time is 5.631 minutes, Hexanal (Hexanal) and the mass-to-charge ratios are 56.05 and 72.10; (2) peak time 8.506 minutes, 1,3,5, 7-cyclooceteteraene (Cyclooctatetraene), mass to charge ratios 51.05, 78.05 and 104.10; (3) peak time 12.290 minutes, Furan, 2-pentyl- (2-n-pentylfuran), mass to charge ratios 53.05, 81.05 and 138.15; (4) the peak-out time is 13.506 minutes, 2,2,5,5-Tetramethyl-3-cyclopenten-1-one (2, 2,5, 5-Tetramethyl-3-cyclopenten-1-one), the mass-to-charge ratio is 70.05, 95.10 and 110.15; (5) peak time 14.071 minutes, Benzene, 1,2, 3-trimethy- (1, 2, 3-trimethylbenzene), mass to charge ratios 104.10 and 120.15; (6) peak time 21.266 minutes, Isophorone (Isophorone), mass to charge ratios 54.05, 82.10 and 138.15; (7) peak time 22.239 minutes, 2,6, 6-trimethy-2-cyclohexene-1, 4-dione (4-oxoisoflurone), mass to charge ratios 68.00, 96.05 and 152.10; (8) peak time 24.096 minutes, 1,3-Cyclohexadiene-1-carboxaldehyde, 2,6, 6-trimethy- (safinaldehyde), mass to charge ratios 91.10, 107.10, 121.15 and 150.15; (9) peak time 25.048 minutes, 4-Methyleneisopherone 4- (Methyleneisophorone), mass to charge ratios 91.05, 107.10 and 150.15; (10) peak time 27.662 minutes, nonaic acid (Nonanoic acid), mass to charge ratios 60.00, 73.05 and 115.10; (11) peak time 30.408 minutes, 2,4,7,9-Tetramethyl-5-decyn-4,7-diol (2, 4,7, 9-Tetramethyl-5-decyne-4, 7-diol), mass to charge ratios 109.10 and 151.15. Characteristic fingerprint as gas chromatography-mass spectrometry of gardenia oil (see fig. 2).
Step (3) identification: taking unknown edible vegetable oil to obtain a gas chromatography-mass spectrometry spectrogram of volatile components of the unknown edible vegetable oil according to the step (1), comparing the characteristic fingerprint (figure 2) of the gas chromatography-mass spectrometry of the gardenia oil with the gas chromatography-mass spectrometry spectrogram of the volatile components of the unknown edible vegetable oil by using a traditional Chinese medicine chromatography fingerprint similarity evaluation system, confirming common characteristic peaks of 11 gardenia and gardenia oil, and distinguishing effective peaks according to the condition that the retention time difference is less than 0.1min, the mass-to-charge ratio difference is less than 0.05 and the relative peak area is more than 0.5 percent, wherein 9 common characteristic peaks appear and are confirmed to be the gardenia oil, and less than 9 common characteristic peaks appear and are confirmed to be the non-gardenia oil.
Fig. 4 is a comparison graph of the gas chromatography mass spectrograms of volatile components of commercially available corn oil, rapeseed oil, peanut oil, camellia oil and soybean oil and the gas chromatography-mass spectrometry characteristic fingerprint spectrogram of gardenia oil, and shows that the number of 11 common characteristic peaks appearing in the gas chromatography mass spectrogram of the volatile components of each finished oil is 3 for corn oil, 3 for rapeseed oil, 4 for peanut oil, 3 for camellia oil and 3 for soybean oil.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (1)
1. A method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrometry fingerprint is characterized in that volatile components of gardenia oil are analyzed and detected by using headspace solid phase microextraction and combining a gas chromatography-mass spectrometry combined technology, a gas chromatography-mass spectrometry characteristic fingerprint of the volatile components of the gardenia oil and the gardenia oil is established, effective peaks of the characteristic fingerprint are compared through evaluation software, and identification of the gardenia oil is achieved;
the method comprises the following steps:
step (1), performing gas chromatography-mass spectrometry analysis on volatile components of the gardenia and the authentic gardenia oil: drying fructus Gardeniae at 70 deg.C, pulverizing, placing 1g fructus Gardeniae powder or 1mL fructus Gardeniae oil in 20mL headspace sample injection bottle, rapidly sealing, inserting 50/30 μm DVB/CAR/PDMS extraction fiber, adsorbing volatile components at 60 deg.C for 40min, pulling out the extraction fiber, rapidly inserting into gas chromatograph sample injection port, desorbing for 5 min, separating and qualitatively analyzing volatile components with gas chromatography-mass spectrometer, retrieving and checking NIST14 LIBRARY standard mass spectrogram of each peak in total ion flow diagram with mass spectrum computer data system, and obtaining gas chromatography-mass spectrometer spectrogram of fructus Gardeniae and authentic volatile components with matching degree greater than 85%;
step (2) establishing a characteristic fingerprint of the gardenia oil volatile component gas chromatography-mass spectrum: according to the gas chromatography-mass spectrometry analysis result of volatile components of the gardenia and the authentic gardenia oil in the step (1), 11 common characteristic peaks of the gardenia and the gardenia oil are selected, (1) the peak time is 5.631 minutes, hexanal and the mass-to-charge ratios are 56.05 and 72.10; (2) peak time 8.506 minutes, cyclooctatetraene, mass to charge ratios 51.05, 78.05, and 104.10; (3) peak time 12.290 minutes, 2-n-pentylfuran, mass to charge ratios 53.05, 81.05, and 138.15; (4) peak time 13.506 minutes, 2,2,5,5-tetramethyl-3-cyclopenten-1-one, mass to charge ratios 70.05, 95.10 and 110.15; (5) peak time 14.071 minutes, 1,2, 3-trimethylbenzene, mass to charge ratios 104.10 and 120.15; (6) peak time 21.266 minutes, isophorone, mass to charge ratios 54.05, 82.10, and 138.15; (7) peak time 22.239 minutes, 4-oxoisofluridone, mass to charge ratios 68.00, 96.05 and 152.10; (8) peak time 24.096 minutes, safranal, mass to charge ratios 91.10, 107.10, 121.15 and 150.15; (9) peak time 25.048 minutes, 4- (methylene isophorone), mass to charge ratios 91.05, 107.10, and 150.15; (10) peak time 27.662 minutes, pelargonic acid, mass to charge ratio 60.00, 73.05 and 115.10; (11) peak time 30.408 minutes, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, mass to charge ratios 109.10 and 151.15; a characteristic fingerprint spectrum of gas chromatography-mass spectrum of gardenia oil;
step (3) identifying gardenia oil: taking the commercial gardenia oil or unknown edible vegetable oil to obtain a gas chromatography-mass spectrum spectrogram of volatile components of the commercial gardenia oil or unknown edible vegetable oil according to the step (1), comparing the characteristic fingerprint of the gas chromatography-mass spectrum of the gardenia oil with the gas chromatography-mass spectrum spectrogram of the volatile components of the commercial gardenia oil or unknown edible vegetable oil by utilizing a traditional Chinese medicine chromatography fingerprint similarity evaluation system, confirming common characteristic peaks of 11 gardenia and gardenia oil, and distinguishing effective peaks according to the condition that the retention time difference is less than 0.1min, the mass-to-charge ratio difference is less than 0.05 and the relative peak area is more than 0.5 percent, wherein 9 common characteristic peaks appear and are confirmed to be gardenia oil, and less than 9 common characteristic peaks appear and are confirmed to be non-gardenia oil;
in the step (1), gas chromatography conditions: chromatographic column, DB-5MS capillary column 30m × 0.25mm × 0.25 μm; temperature programming: maintaining at 40 deg.C for 4min, heating to 70 deg.C at 6 deg.C/min, maintaining for 8 min, heating to 180 deg.C at 6 deg.C/min, and maintaining for 3 min; the temperature of a sample inlet is 250 ℃; carrier gas He with the flow rate of 1 mL/min; no flow separation, solvent delay 4 min;
in the step (1), mass spectrum conditions are as follows: EI ion source, electron energy 70eV, scanning range m/z50.00-500.00, ion source temperature 200 deg.C, interface temperature 250 deg.C.
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