CN110927283A - Detection method for identifying natural garlic oil adulterated with synthetic garlic oil - Google Patents
Detection method for identifying natural garlic oil adulterated with synthetic garlic oil Download PDFInfo
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- CN110927283A CN110927283A CN201911283653.4A CN201911283653A CN110927283A CN 110927283 A CN110927283 A CN 110927283A CN 201911283653 A CN201911283653 A CN 201911283653A CN 110927283 A CN110927283 A CN 110927283A
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- garlic oil
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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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Abstract
The invention discloses a detection method for identifying natural garlic oil adulterated with synthetic garlic oil, belonging to the technical field of food detection. The invention utilizes trace 1, 5-hexadiene contained in the synthetic garlic oil, adopts gas chromatography-mass spectrometry to detect, and carries out qualitative library retrieval on a mass spectrogram, so that the content of 1, 5-hexadiene is determined, and the adulterated synthetic garlic oil in the natural garlic oil can be determined. The method has the advantages of simple pretreatment operation, simple data processing and simple adulteration judging mode.
Description
Technical Field
The invention belongs to the technical field of food detection, and particularly relates to a detection method for identifying natural garlic oil adulterated with synthetic garlic oil.
Background
The natural garlic oil is prepared from garlic through washing, mashing tissue, extracting, filtering and distilling. Since the garlic oil contains a large amount of organic thioether components with medicinal value and also contains a small amount of carbohydrate and nearly 20 components such as amino acid, iron, selenium and the like which are beneficial to the health of human bodies, the garlic oil is widely applied to medical sanitation, health care and food industry. However, the production cost of converting garlic into garlic oil is very high, and the conversion rate is less than 1%. Therefore, synthetic garlic oil has been used in some fields as a supplement and substitute for high-value natural garlic oil, but is unsuitable for use in the food field because of a small amount of chemical residues contained in the synthetic garlic oil. Illegal merchants adopt synthetic garlic oil or mix the synthetic garlic oil and natural garlic oil to serve as natural garlic oil in order to earn benefits.
Disclosure of Invention
The invention aims to provide a detection method for identifying natural garlic oil adulterated with synthetic garlic oil.
The detection method is a gas chromatography mass spectrometry method, and the gas chromatography mass spectrograms of the natural garlic oil and the synthetic garlic oil are compared to find that trace 1, 5-hexadiene exists in the synthetic garlic oil but does not exist in the natural garlic oil. Therefore, a detection method for identifying the adulterated synthetic garlic oil in the natural garlic oil is established.
The specific detection operation steps are as follows:
(1) establishing gas chromatography mass spectrogram of natural garlic oil
Establishing a gas chromatography mass spectrogram of the natural garlic oil by a gas chromatography-mass spectrometry method;
(2) establishing gas chromatography mass spectrogram of synthetic garlic oil
Detecting the garlic oil to be detected by a gas chromatography-mass spectrometry method to obtain a gas chromatography mass spectrogram of the garlic oil to be detected;
(3) comparison of
Comparing the gas chromatography mass spectrogram of the natural garlic oil with the gas chromatography mass spectrogram of the tested garlic oil, wherein if the tested garlic oil is detected to contain 1, 5-hexadiene, the tested garlic oil is synthetic garlic oil; if the detected garlic oil does not detect that the garlic oil contains 1, 5-hexadiene, the detected garlic oil is natural garlic oil.
The detection conditions of the gas chromatography-mass spectrometry are further defined as follows:
DB-5MS capillary column, 30 m × 0.25 mm × 0.25 μm; preparing a search spectrum library; the chromatographic analysis conditions were: the temperature of a sample inlet is 100 ℃, helium is used as carrier gas, the flow rate is 1.0 mL/min, the split ratio is 100:1, and the sample introduction amount is 1 muL; the temperature programming conditions are as follows: the initial temperature is 45 ℃, the temperature is increased to 80 ℃ at 5 ℃/min, then the temperature is increased to 180 ℃ at 20 ℃/min, and the temperature is kept for 12 min; the ion source is an EI source with an energy of 70 eV.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the method has simple pretreatment operation, and can directly dilute the detected garlic oil for sample injection.
2. The method has simple data processing, and only needs to carry out spectrum library retrieval on the mass spectrogram.
3. The method of the invention has simple adulteration judging mode, and the adulteration of the synthetic garlic oil in the natural garlic oil can be proved only by searching the spectrogram to contain 1, 5-hexadiene.
Detailed Description
The present invention will be further described with reference to the following examples.
Examples
Diluting garlic oil by 100 times with n-hexane, directly injecting sample, measuring total ion flow diagram by gas chromatography mass spectrometry, and retrieving mass spectrogram by using a retrieval library. When the mass spectrogram detects 1, 5-hexadiene, the natural garlic oil is proved to be adulterated with the synthetic garlic oil.
The specific detection conditions of the gas chromatography-mass spectrometry method are as follows:
DB-5MS capillary column, 30 m × 0.25 mm × 0.25 μm; preparing a search spectrum library; the chromatographic analysis conditions were: the temperature of a sample inlet is 100 ℃, helium is used as carrier gas, the flow rate is 1.0 mL/min, the split ratio is 100:1, and the sample introduction amount is 1 muL; the temperature programming conditions are as follows: the initial temperature is 45 ℃, the temperature is increased to 80 ℃ at the speed of 5 ℃/min, then the temperature is increased to 180 ℃ at the speed of 20 ℃/min, and the temperature is kept for 12 min; the ion source is an EI source with an energy of 70 eV.
Claims (2)
1. A detection method for identifying natural garlic oil adulterated with synthetic garlic oil is characterized by comprising the following operation steps:
(1) establishing gas chromatography mass spectrogram of natural garlic oil
Establishing a gas chromatography mass spectrogram of the natural garlic oil by a gas chromatography-mass spectrometry method;
(2) establishing gas chromatography mass spectrogram of synthetic garlic oil
Detecting the garlic oil to be detected by a gas chromatography-mass spectrometry method to obtain a gas chromatography mass spectrogram of the garlic oil to be detected;
(3) comparison of
Comparing the gas chromatography mass spectrogram of the natural garlic oil with the gas chromatography mass spectrogram of the tested garlic oil, wherein if the tested garlic oil is detected to contain 1, 5-hexadiene, the tested garlic oil is synthetic garlic oil; if the detected garlic oil does not detect that the garlic oil contains 1, 5-hexadiene, the detected garlic oil is natural garlic oil.
2. The assay method according to claim 1, wherein the assay method comprises the following steps:
the detection conditions of the gas chromatography-mass spectrometry are as follows:
DB-5MS capillary column, 30 m × 0.25 mm × 0.25 μm; preparing a search spectrum library; the chromatographic analysis conditions were: the temperature of a sample inlet is 100 ℃, helium is used as carrier gas, the flow rate is 1.0 mL/min, the split ratio is 100:1, and the sample introduction amount is 1 muL; the temperature programming conditions are as follows: the initial temperature is 45 ℃, the temperature is increased to 80 ℃ at 5 ℃/min, then the temperature is increased to 180 ℃ at 20 ℃/min, and the temperature is kept for 12 min; the ion source is an EI source with an energy of 70 eV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911283653.4A CN110927283A (en) | 2019-12-13 | 2019-12-13 | Detection method for identifying natural garlic oil adulterated with synthetic garlic oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911283653.4A CN110927283A (en) | 2019-12-13 | 2019-12-13 | Detection method for identifying natural garlic oil adulterated with synthetic garlic oil |
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| CN110927283A true CN110927283A (en) | 2020-03-27 |
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| CN201911283653.4A Pending CN110927283A (en) | 2019-12-13 | 2019-12-13 | Detection method for identifying natural garlic oil adulterated with synthetic garlic oil |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR940020117A (en) * | 1993-02-01 | 1994-09-15 | 김기운 | New Analysis of Allicin in Garlic Oil |
| CN101337917A (en) * | 2008-08-08 | 2009-01-07 | 淮阴工学院 | Method for catalytic synthesis of garlic oil of different combinations by phase-transfer method |
| CN101691346A (en) * | 2009-09-08 | 2010-04-07 | 北京资源亚太饲料科技有限公司 | Separation and purification method of synthetic garlic oil |
| US20140314729A1 (en) * | 2013-04-12 | 2014-10-23 | Creative Medical Health Inc. | Nutraceutical formulation for treatment of elevated cholesterol and cardiovascular disease |
-
2019
- 2019-12-13 CN CN201911283653.4A patent/CN110927283A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR940020117A (en) * | 1993-02-01 | 1994-09-15 | 김기운 | New Analysis of Allicin in Garlic Oil |
| CN101337917A (en) * | 2008-08-08 | 2009-01-07 | 淮阴工学院 | Method for catalytic synthesis of garlic oil of different combinations by phase-transfer method |
| CN101691346A (en) * | 2009-09-08 | 2010-04-07 | 北京资源亚太饲料科技有限公司 | Separation and purification method of synthetic garlic oil |
| US20140314729A1 (en) * | 2013-04-12 | 2014-10-23 | Creative Medical Health Inc. | Nutraceutical formulation for treatment of elevated cholesterol and cardiovascular disease |
Non-Patent Citations (4)
| Title |
|---|
| HM SEO 等: "Volatile Flavor Compounds of Freeze Dried Garlic and Garlic Roasted with Oils", 《JOURNAL OF THE KOREAN SOCIETY OF FOOD SCIENCE AND NUTRITION》 * |
| 王建 等: "大蒜油及其软胶囊中二烯丙基三硫醚等硫醚类化合物的分析 ", 《中国卫生检验杂志》 * |
| 郑屏 等: "天然大蒜油及合成大蒜素的气相色谱-质谱分析 ", 《分析化学》 * |
| 陶宁萍 等: "顶空固相微萃取气质联用测定蒜油挥发性成分", 《食品工业科技》 * |
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Application publication date: 20200327 |