CN108680669A - The test method of anthraquinone in a kind of plant-derived product and food - Google Patents
The test method of anthraquinone in a kind of plant-derived product and food Download PDFInfo
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- CN108680669A CN108680669A CN201810432774.XA CN201810432774A CN108680669A CN 108680669 A CN108680669 A CN 108680669A CN 201810432774 A CN201810432774 A CN 201810432774A CN 108680669 A CN108680669 A CN 108680669A
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- anthraquinone
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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 kind of test methods of anthraquinone in plant-derived product and food to be included the following steps using gas-chromatography tandem mass spectrometry：Sample is weighed, 5 20mL of acetone is added, be fully vortexed 2min, shaken overnight, centrifugation, supernatant is taken, it is to be clean, it takes and has activated GCB pillars, above-mentioned supernatant is added, finally eluted with 3 10mL acetone, elution liquid nitrogen, which is blown, closely to be done, and with 1mL acetone constant volumes, crosses film, examination with computer.The present invention can simultaneously suitable for the plant-derived product such as tealeaves, matrimony vine, spirulina anthraquinone residue gas-chromatography tandem mass spectrometry, detection be limited to 0.005mg/kg.
Description
Technical field
The present invention relates to a kind of test method, more particularly to the test side of anthraquinone in a kind of plant-derived product and food
Method.
Background technology
So far, it not can be adapted for the detection method of anthraquinone residual quantity in tealeaves, can not detect Chinese holly yet
The detection method of anthraquinone residual quantity in the products such as Qi, spirulina, even if remote if with reference to its detection limit of the national standard of other similar methods
Far above 0.005mg/kg.
Invention content
To solve the problems, such as above-mentioned background technology, the purpose of the present invention is to provide a kind of plant-derived product and
The test method of anthraquinone in food, with reach being capable of the anthraquinone suitable for the plant-derived product such as tealeaves, matrimony vine, spirulina simultaneously
The gas-chromatography tandem mass spectrometry of residue, detection are limited to the purpose of 0.005mg/kg.
In order to achieve the above objectives, technical scheme is as follows：
The test method of anthraquinone in a kind of plant-derived product and food, using gas-chromatography tandem mass spectrometry, including with
Lower step：
Sample is weighed, acetone 5-20mL is added, be fully vortexed 2min, shaken overnight, and centrifugation takes supernatant, to be clean, takes
GCB pillars have been activated, above-mentioned supernatant is added, finally 3-10mL acetone have been used to elute, elution liquid nitrogen, which is blown, closely to be done, fixed with 1mL acetone
Hold, crosses film, examination with computer.
Preferably, the chromatographic column of the gas-chromatography tandem mass spectrometer in the gas-chromatography tandem mass spectrometry is HP-5MS,
Carrier gas is high-purity helium 99.9999%.
Preferably, the ion source of the gas-chromatography tandem mass spectrometer is EI+, and injector temperature is 280 DEG C, flow velocity
1.0ml/min, injection port can be divided into shunting and not shunt.
Preferably, the sample size of the gas-chromatography tandem mass spectrometer is 1ul, and transmission line temperature is 280 DEG C, ion source temperature
Degree is 300 DEG C, and quadrupole rod temperature is 180 DEG C, and retention time is locked as chlorpyrifos-methyl lock 18.111min.
Preferably, the temperature program of the gas-chromatography tandem mass spectrometer is that 1min40 DEG C/min of 60 DEG C of holdings rises to 120
DEG C, it keeps 5 DEG C/min of 0.1min to rise to 310 DEG C, is kept for 0min total times 40.5min.
Through the above technical solutions, in a kind of plant-derived product provided by the invention and food anthraquinone test method,
By acetone extraction target substance, after Solid Phase Extraction column purification, GC-MS is tested, can be suitable for simultaneously tealeaves, matrimony vine,
The gas-chromatography tandem mass spectrometry of anthraquinone residue in the plant-derived product such as spirulina, detection are limited to 0.005mg/kg.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below.
The test method of anthraquinone in a kind of plant-derived product and food provided by the invention, using gas-chromatography series connection matter
Spectrometry includes the following steps：
Sample is weighed, acetone 5-20mL is added, be fully vortexed 2min, shaken overnight, and centrifugation takes supernatant, to be clean, takes
GCB pillars have been activated, above-mentioned supernatant is added, finally 3-10mL acetone have been used to elute, elution liquid nitrogen, which is blown, closely to be done, fixed with 1mL acetone
Hold, crosses film, examination with computer.
The chromatographic column of gas-chromatography tandem mass spectrometer in the gas-chromatography tandem mass spectrometry is HP-5MS, and carrier gas is height
Pure helium 99.9999%, ion source EI+, injector temperature are 280 DEG C, and flow velocity 1.0ml/min, injection port can be divided into shunting
It does not shunt, sample size 1ul, transmission line temperature is 280 DEG C, and ion source temperature is 300 DEG C, and quadrupole rod temperature is 180 DEG C, is protected
It is that chlorpyrifos-methyl locks 18.111min to stay time lock.
The temperature program of the gas-chromatography tandem mass spectrometer is 60 DEG C and 1min40 DEG C/min is kept to rise to 120 DEG C, keeps
5 DEG C/min of 0.1min rise to 310 DEG C, are kept for 0min total times 40.5min.
The test method of anthraquinone, passes through acetone extraction object in a kind of plant-derived product and food disclosed by the invention
Matter, after Solid Phase Extraction column purification, GC-MS is tested, and can be suitable for the plant-derived productions such as tealeaves, matrimony vine, spirulina simultaneously
The gas-chromatography tandem mass spectrometry of anthraquinone residue in product, detection are limited to 0.005mg/kg.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (5)
1. the test method of anthraquinone in a kind of plant-derived product and food, using gas-chromatography tandem mass spectrometry, feature exists
In including the following steps：
Sample is weighed, acetone 5-20mL is added, be fully vortexed 2min, shaken overnight, and centrifugation takes supernatant, to be clean, takes and has lived
Change GCB pillars, are added above-mentioned supernatant, finally 3-10mL acetone are used to elute, and elution liquid nitrogen, which is blown, closely to be done, with 1mL acetone constant volumes, mistake
Film, examination with computer.
2. the test method of anthraquinone in a kind of plant-derived product according to claim 1 and food, which is characterized in that institute
The chromatographic column for stating the gas-chromatography tandem mass spectrometer in gas-chromatography tandem mass spectrometry is HP-5MS, and carrier gas is high-purity helium
99.9999%.
3. the test method of anthraquinone in a kind of plant-derived product according to claim 2 and food, which is characterized in that institute
The ion source for stating gas-chromatography tandem mass spectrometer is EI+, and injector temperature is 280 DEG C, flow velocity 1.0ml/min.
4. the test method of anthraquinone in a kind of plant-derived product according to claim 3 and food, which is characterized in that institute
The sample size for stating gas-chromatography tandem mass spectrometer is 1ul, and transmission line temperature is 280 DEG C, and ion source temperature is 300 DEG C, quadrupole rod
Temperature is 180 DEG C, and retention time is locked as chlorpyrifos-methyl lock 18.111min.
5. the test method of anthraquinone in a kind of plant-derived product according to claim 3 and food, which is characterized in that institute
The temperature program for stating gas-chromatography tandem mass spectrometer is 60 DEG C and 1min40 DEG C/min kept to rise to 120 DEG C, keep 5 DEG C of 0.1min/
Min rises to 310 DEG C, is kept for 0min total times 40.5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810432774.XA CN108680669A (en) | 2018-05-08 | 2018-05-08 | The test method of anthraquinone in a kind of plant-derived product and food |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810432774.XA CN108680669A (en) | 2018-05-08 | 2018-05-08 | The test method of anthraquinone in a kind of plant-derived product and food |
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| CN108680669A true CN108680669A (en) | 2018-10-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810432774.XA Pending CN108680669A (en) | 2018-05-08 | 2018-05-08 | The test method of anthraquinone in a kind of plant-derived product and food |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117420256A (en) * | 2023-10-16 | 2024-01-19 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424855A (en) * | 2015-11-23 | 2016-03-23 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring residual amount of anthraquinone in tea with gas chromatography-mass spectrum/mass spectrum method |
-
2018
- 2018-05-08 CN CN201810432774.XA patent/CN108680669A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424855A (en) * | 2015-11-23 | 2016-03-23 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring residual amount of anthraquinone in tea with gas chromatography-mass spectrum/mass spectrum method |
Non-Patent Citations (2)
| Title |
|---|
| KOKILA, K 等: "Isolation, identification and biological applications of anthraquinone (methylated rhein) from Albizia saman seed extracts.", 《JOURNAL OF FOOD PROCESSING AND PRESERVATION》 * |
| 黄秋研 等: "固相萃取-气相色谱-质谱法测定茶叶中蒽醌残留", 《广东化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117420256A (en) * | 2023-10-16 | 2024-01-19 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
| CN117420256B (en) * | 2023-10-16 | 2024-06-04 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
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Application publication date: 20181019 |