CN108776182A - One kind is for food and the how remaining detection method of hormone in health food - Google Patents
One kind is for food and the how remaining detection method of hormone in health food Download PDFInfo
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- CN108776182A CN108776182A CN201810432773.5A CN201810432773A CN108776182A CN 108776182 A CN108776182 A CN 108776182A CN 201810432773 A CN201810432773 A CN 201810432773A CN 108776182 A CN108776182 A CN 108776182A
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- food
- methanol
- liquid chromatography
- hormone
- detection method
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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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention discloses one kind to be as follows for food and the how remaining detection method of hormone in health food using liquid chromatography tandem mass spectrometry, including extraction, purification, three step of examination with computer：By taking animal derived food as an example, 1) extraction, it weighs sample and has in plug plastic centrifuge tube in 50mL, ammonium acetate buffer solution is added, 5-20mL methanol ultrasonic extractions, centrifugation is added in vortex mixing, supernatant is transferred in centrifuge tube, repeats to extract once, it is to be clean to merge supernatant；2) it purifies, above-mentioned supernatant is splined on to the HLB solid-phase extraction columns activated, it is eluted with 3-10mL water, methanol, pillar is drained, it is eluted with 3-10mL dichloro methane-methanols and collects eluent, liquid nitrogen drying is eluted, with 1mL methanol-water solution dissolved residues, is measured for liquid chromatography-mass spectrography/mass spectrum；3) examination with computer.The present invention is easy to operate, takes short, saving testing cost.
Description
Technical field
The present invention relates to a kind of detection methods, more particularly to a kind of for food and the how remaining inspection of hormone in health food
Survey method.
Background technology
Currently, for the residual of drug in health food, general elder generation's thin-layer qualitative, then liquid chromatography qualitative detection, finally
When the positive detects, using mass spectrum confirmation, but above method step is long, takes time and effort, and complex pretreatment, not easy to operate,
A variety of medicament residues cannot be identified simultaneously.
Invention content
To solve the problems, such as above-mentioned background technology, the purpose of the present invention is to provide one kind being used for food and health care
The how remaining detection method of hormone in food, it is easy to operate to reach method, it is time-consuming short, save the purpose of testing cost.
In order to achieve the above objectives, technical scheme is as follows：
One kind is for the how remaining detection method of hormone in food and health food, using liquid chromatography tandem mass spectrometry,
Including extraction, purification, three step of examination with computer, it is as follows：
Animal derived food
1) it extracts, weighs sample and have in plug plastic centrifuge tube in 50mL, ammonium acetate buffer solution is added, vortex mixing adds
Enter 5-20mL methanol ultrasonic extractions, centrifuge, supernatant is transferred in centrifuge tube, repeats to extract once, it is to be clean to merge supernatant；
2) it purifies, above-mentioned supernatant is splined on to the HLB solid-phase extraction columns activated, eluted with 3-10mL water, methanol, it will
Pillar is drained, and eluent, elution liquid nitrogen drying, with 1mL methanol-waters are eluted and collected with 3-10mL dichloro methane-methanols
Solution dissolved residue is measured for liquid chromatography-mass spectrography/mass spectrum；
3) examination with computer；
Healthcare food
1) it extracts, weighs sample in 50mL centrifuge tubes, 10-40mL methanol-waters are added, be capped mixing, ultrasound has extracted
Finish postcooling to room temperature, be transferred to 100mL volumetric flasks, be used in combination methanol-water to be settled to uniformly mixed, take 1.0mL, film is crossed, for liquid phase
Chromatography-mass spectroscopy is measured.
Preferably, the healthcare food includes tablet, capsule, biscuit, coffee, tealeaves and powder sample.
Preferably, the healthcare food further includes oral solution, step be pipette 1-10mL liquor samples in
In 100mL volumetric flasks, it is settled to scale with methanol-water, is uniformly mixed, film is crossed, is measured for liquid chromatography mass/mass spectrum.
Preferably, the positive ion mode chromatographic column of the Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry
For Agilent chromatographic columns, 2.7 μm, size is 3.0mm × 100mm.
Preferably, the mobile phase of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：A：0.1% formic acid water, B：0.1% formic acid second
Nitrile, flow velocity 0.4mL/min, column temperature are 35 DEG C, and sample size is 10 μ L.
Preferably, the Mass Spectrometry Conditions of the Liquid Chromatography-Tandem Mass Spectrometry instrument are：A) ion source：Electric spray ion source；B) it sweeps
Retouch mode：Cation scans；C) detection mode：More reaction detections；D) dry temperature degree：200℃；E) dry gas stream speed：14L/
min；F) sheath temperature degree：250℃；G) sheath gas：11L/min；H) voltage of transfer capillary：3000V；I) atomizer pressure
Power：25psi.
Through the above technical solutions, provided by the invention a kind of for food and the how remaining detection of hormone in health food
Method, target compound in animal derived food is through enzymolysis, with extraction solution extraction, through Solid phase extraction, liquid chromatogram
Tandem mass spectrometer measures；Target compound through being extracted with extraction solution, survey by purification, Liquid Chromatography-Tandem Mass Spectrometry instrument in health food
Fixed, the above method is easy to operate, it is short to take, saves testing cost, and the residual detection of all drug is limited in food after detection
0.4 μ g/kg, in health food all drug residual detections be limited to 1mg/kg.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below.
It is provided by the invention a kind of for food and the how remaining detection method of hormone in health food, using liquid chromatogram
Tandem mass spectrometry, including extraction, purification, three step of examination with computer, are as follows：
By taking animal derived food as an example, including tablet, capsule, biscuit, coffee, tealeaves and powder sample
1) it extracts, weighs sample and have in plug plastic centrifuge tube in 50mL, ammonium acetate buffer solution is added, vortex mixing adds
Enter 5-20mL methanol ultrasonic extractions, centrifuge, supernatant is transferred in centrifuge tube, repeats to extract once, it is to be clean to merge supernatant；
2) it purifies, above-mentioned supernatant is splined on to the HLB solid-phase extraction columns activated, eluted with 3-10mL water, methanol, it will
Pillar is drained, and eluent, elution liquid nitrogen drying, with 1mL methanol-waters are eluted and collected with 3-10mL dichloro methane-methanols
Solution dissolved residue is measured for liquid chromatography-mass spectrography/mass spectrum；
3) examination with computer；
By taking healthcare food as an example
1) it extracts, weighs sample in 50mL centrifuge tubes, 10-40mL methanol-waters are added, be capped mixing, ultrasound has extracted
Finish postcooling to room temperature, be transferred to 100mL volumetric flasks, be used in combination methanol-water to be settled to uniformly mixed, take 1.0mL, film is crossed, for liquid phase
Chromatography-mass spectroscopy is measured.
Healthcare food further includes oral solution, and step is to pipette 1-10mL liquor samples in 100mL volumetric flasks
In, it is settled to scale with methanol-water, is uniformly mixed, film is crossed, is measured for liquid chromatography mass/mass spectrum.
The positive ion mode chromatographic column of Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry is
Agilent chromatographic columns, 2.7 μm, size is 3.0mm × 100mm, and the mobile phase of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：A：
0.1% formic acid water, B：0.1% formic acid acetonitrile, flow velocity 0.4mL/min, column temperature are 35 DEG C, and sample size is 10 μ L, the liquid
The mass spectrometric Mass Spectrometry Conditions of phase chromatographic tandem are：A) ion source：Electric spray ion source；B) scan mode：Cation scans；c)
Detection mode：More reaction detections；D) dry temperature degree：200℃；E) dry gas stream speed：14L/min；F) sheath temperature degree： 250
℃；G) sheath gas：11L/min；H) voltage of transfer capillary：3000V；I) nebulizer pressure：25psi, gradient elution
Condition such as following table：
Table 1 is condition of gradient elution
| Time/min | 0.1% formic acid water | 0.1% formic acid acetonitrile |
| 0-1 | 95 | 5 |
| 1.5-2.5 | 70 | 30 |
| 3-5 | 30 | 70 |
| 5.5-8.5 | 0 | 100 |
| 9-12 | 95 | 5 |
Liquid Chromatography-Tandem Mass Spectrometry instrument can also use negative ion mode, and mobile phase is distinguished as with positive ion mode：
A：20mmol/L ammonium acetates, B：Acetonitrile, scan mode scan for anion, condition of gradient elution such as following table：
Table 2 is condition of gradient elution
| Time/min | 20mmol/L ammonium acetates | Acetonitrile |
| 0-1 | 95 | 5 |
| 1.5-2.8 | 60 | 40 |
| 3-4 | 20 | 80 |
| 4.5-6.5 | 0 | 100 |
| 7-10 | 95 | 5 |
It is disclosed by the invention a kind of for food and the how remaining detection method of hormone in health food, animal derived food
In target compound through enzymolysis, with extraction solution extraction, through Solid phase extraction, Liquid Chromatography-Tandem Mass Spectrometry instrument measures；It protects
Through being extracted with extraction solution, purification, Liquid Chromatography-Tandem Mass Spectrometry instrument measures target compound in health food, above method operation letter
Just short, saving testing cost, is taken, the residual detection of all drug is limited to 0.4 μ g/kg, health food in food after detection
In the residual detection of all drug be limited to 1mg/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 (6)
1. one kind is for food and the how remaining detection method of hormone in health food, using liquid chromatography tandem mass spectrometry, packet
Include extraction, purification, three step of examination with computer, which is characterized in that be as follows：
Animal derived food
1) it extracts, weighs sample and have in plug plastic centrifuge tube in 50mL, ammonium acetate buffer solution is added, 5- is added in vortex mixing
20mL methanol ultrasonic extractions, centrifugation, supernatant is transferred in centrifuge tube, repeats to extract once, it is to be clean to merge supernatant；
2) it purifies, above-mentioned supernatant is splined on to the HLB solid-phase extraction columns activated, eluted with 3-10mL water, methanol, by pillar
It drains, eluent, elution liquid nitrogen drying, with 1mL methanol-water solutions is eluted and collected with 3-10mL dichloro methane-methanols
Dissolved residue is measured for liquid chromatography-mass spectrography/mass spectrum；
3) examination with computer；
Healthcare food
1) it extracts, weighs sample in 50mL centrifuge tubes, 10-40mL methanol-waters are added, be capped mixing, ultrasound, after extraction
It is cooled to room temperature, is transferred to 100mL volumetric flasks, be used in combination methanol-water to be settled to uniformly mixed, take 1.0mL, film is crossed, for liquid phase color
Spectrum-mass spectrum is measured.
2. according to claim 1 a kind of for food and the how remaining detection method of hormone in health food, feature
It is, the healthcare food includes tablet, capsule, biscuit, coffee, tealeaves and powder sample.
3. according to claim 1 a kind of for food and the how remaining detection method of hormone in health food, feature
It is, the healthcare food further includes oral solution, and step is to pipette 1-10mL liquor samples in 100mL volumetric flasks
In, it is settled to scale with methanol-water, is uniformly mixed, film is crossed, is measured for liquid chromatography mass/mass spectrum.
4. according to claim 1 a kind of for food and the how remaining detection method of hormone in health food, feature
It is, the positive ion mode chromatographic column of the Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry is Agilent
Chromatographic column, 2.7 μm, size is 3.0mm × 100mm.
5. according to claim 4 a kind of for food and the how remaining detection method of hormone in health food, feature
It is, the mobile phase of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：A：0.1% formic acid water, B：0.1% formic acid acetonitrile, flow velocity are
0.4mL/min, column temperature are 35 DEG C, and sample size is 10 μ L.
6. according to claim 5 a kind of for food and the how remaining detection method of hormone in health food, feature
It is, the Mass Spectrometry Conditions of the Liquid Chromatography-Tandem Mass Spectrometry instrument are：A) ion source：Electric spray ion source；B) scan mode：Just from
Son scanning；C) detection mode：More reaction detections；D) dry temperature degree：200℃；E) dry gas stream speed：14L/min；F) sheath temperature
Degree：250℃；G) sheath gas：11L/min；H) voltage of transfer capillary：3000V；I) nebulizer pressure：25psi.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810432773.5A CN108776182A (en) | 2018-05-08 | 2018-05-08 | One kind is for food and the how remaining detection method of hormone in health food |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN201810432773.5A CN108776182A (en) | 2018-05-08 | 2018-05-08 | One kind is for food and the how remaining detection method of hormone in health food |
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| CN108776182A true CN108776182A (en) | 2018-11-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113324978A (en) * | 2021-06-01 | 2021-08-31 | 天津市食品安全检测技术研究院 | Method for detecting calcium and iron in health food |
| CN116990421A (en) * | 2023-09-27 | 2023-11-03 | 深圳市检验检疫科学研究院 | Method for detecting residual quantity of nosiheptide in animal-derived food |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749270A (en) * | 2013-12-27 | 2015-07-01 | 内蒙古出入境检验检疫局检验检疫技术中心 | Method for simultaneously detecting two glucocorticoid isomerides in animal-derived food |
-
2018
- 2018-05-08 CN CN201810432773.5A patent/CN108776182A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749270A (en) * | 2013-12-27 | 2015-07-01 | 内蒙古出入境检验检疫局检验检疫技术中心 | Method for simultaneously detecting two glucocorticoid isomerides in animal-derived food |
Non-Patent Citations (2)
| Title |
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| 崔晓亮 等: "超高效液相色谱-串联电喷雾四极杆质谱法同时测定牛奶中12种糖皮质激素的残留", 《色谱》 * |
| 邹晓春 等: "高效液相色谱-串联质谱法同时测定肉类食品中5种肾上腺皮质激素", 《中国卫生检验杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113324978A (en) * | 2021-06-01 | 2021-08-31 | 天津市食品安全检测技术研究院 | Method for detecting calcium and iron in health food |
| CN113324978B (en) * | 2021-06-01 | 2023-08-01 | 天津市食品安全检测技术研究院 | Method for detecting calcium and iron in health food |
| CN116990421A (en) * | 2023-09-27 | 2023-11-03 | 深圳市检验检疫科学研究院 | Method for detecting residual quantity of nosiheptide in animal-derived food |
| CN116990421B (en) * | 2023-09-27 | 2023-12-05 | 深圳市检验检疫科学研究院 | Method for detecting residual quantity of nosiheptide in animal-derived food |
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Application publication date: 20181109 |