CN108333275A - A kind of method that LC-MS/MS measures the putrescine in soy sauce - Google Patents
A kind of method that LC-MS/MS measures the putrescine in soy sauce Download PDFInfo
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- CN108333275A CN108333275A CN201810412022.7A CN201810412022A CN108333275A CN 108333275 A CN108333275 A CN 108333275A CN 201810412022 A CN201810412022 A CN 201810412022A CN 108333275 A CN108333275 A CN 108333275A
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- China
- Prior art keywords
- putrescine
- soy sauce
- measures
- ion pair
- concentration
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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
Abstract
The invention discloses a kind of methods that LC MS/MS measure the putrescine in soy sauce, are monitored using reaction of high order, and quantitative with ion pair 89.2=＞ 72.1, ion pair 89.2=＞ 55.1 are qualitative, direct injection analysis after soy sauce dilution.The present invention has the features such as easy to operate, testing cost is low, and the range of linearity is wide, the high feature of the rate of recovery, has very wide application range.
Description
Technical field
The present invention relates to a kind of food composition analysis fields, and in particular to putrescine detection method in a kind of soy sauce.
Background technology
Putrescine is one kind of biogenic amine, be against the wind it is smelly go out it is several it is inner ground super dead bomb, in air concentration reach tens
Ppm can swoon people to smoked, there is severe toxicity.Putrescine is that food is formed by ornithine decarboxylation during the fermentation.In sauce fermentation
In the process, there is a large amount of ornithine, some putrescine can be generated in the effect of microorganism, soy sauce.Therefore, the color in soy sauce is detected
Amine is particularly significant.Currently used method is to be detected with liquid phase after putrescine derivatization, but this method is time-consuming longer.The present invention is logical
After diluting soy sample, using the putrescine content in reaction of high order monitoring (MRM) analysis soy sauce.
Invention content
It is an object of the present invention to the problem of overcoming the complex pretreatment of the prior art, provide rotten in a kind of soy sauce
The identification method of amine.
The invention is realized by the following technical scheme：
1 chromatographic condition, mobile phase A：0.1% aqueous formic acid；Mobile phase B：0.1% formic acid acetonitrile solution.0min,
5%B；5min, 20%B.
2 Mass Spectrometry Conditions：Using electric spray ion source, 300 DEG C, flow velocity 8L/min, capillary voltage 4000V of gas temperature,
Positive ion mode.Fragmentation voltage 45, fragmentation voltage 9, accelerating potential 4, quota ion pair 89.2=＞ 72.1；Fragmentation voltage 45,
Fragmentation voltage 21, accelerating potential 4, qualitative ion pair 89.2=＞ 55.1.
3 weigh a certain amount of tryptamines standard items, prepare the standard solution of certain gradient, carry out LC-MS/MS analyses.
4. soy sample dilutes 400-1000 times, direct injection analysis.
5. integral retention time is 1.023min peak areas, calibration curve is determined.The retention time for bringing sample into is
1.023min peak areas calculate concentration × extension rate, i.e. the putrescine content of soy sauce.
Description of the drawings
Attached drawing is the matched curve in embodiment 1.
Specific implementation mode：
Technical scheme of the present invention is described further below by specific embodiment：
Embodiment 1
1 chromatographic condition, mobile phase A：0.1% aqueous formic acid；Mobile phase B：0.1% formic acid acetonitrile solution.0min,
5%B；5min, 20%B, using C3 reverse-phase chromatographic columns.
2 Mass Spectrometry Conditions：Using electric spray ion source, 300 DEG C, flow velocity 8L/min, capillary voltage 4000V of gas temperature,
Positive ion mode.Fragmentation voltage 45, collision energy 9, accelerating potential 4, quota ion pair 89.2=＞ 72.1；Fragmentation voltage 45,
Collision energy 21, accelerating potential 4, qualitative ion pair 89.2=＞ 55.1.
3 weigh a certain amount of putrescine standard items, prepare 7 μ g/L, 35.1 μ g/L, 175.4 μ g/L, and the standard of 877.2 μ g/L is molten
Liquid, sample size are 5 μ L, carry out LC-MS/MS analyses.Integral retention time is 1.023min peak areas, obtains calibration curve y=
602.95x+21184 R2=0.995 wherein y are peak area, x is Putrescine concentration.
4. soy sample dilutes 1000 times, sample size is 5 μ L.
5. the retention time for bringing sample into is 1.023min peak areas 274170, according to calibration curve, it is 423.8 μ g/ to obtain x
L calculates concentration × extension rate, i.e., tryptamines content 423.8mg/L in soy sauce.
This method uses dilution method, eliminates sodium chloride to mass spectrographic influence, direct injected avoids cumbersome after dilution
Pre-treatment.The wide 1 μ g/L-900 μ g/L of the range of linearity, mark-on reclaims are between 80%-93%.
Claims (1)
1. a kind of method that LC-MS/MS measures putrescine in soy sauce, it is characterised in that：Using the diluted method of soy sauce, quota ion
To 89.2=＞ 72.1；Qualitative ion pair 89.2=＞ 55.1.Gradient concentration is done with putrescine standard items, liquid matter analysis is carried out, obtains
To matched curve, the concentration of putrescine in soy sauce is calculated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810412022.7A CN108333275A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the putrescine in soy sauce |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810412022.7A CN108333275A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the putrescine in soy sauce |
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| CN108333275A true CN108333275A (en) | 2018-07-27 |
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| CN201810412022.7A Pending CN108333275A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the putrescine in soy sauce |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51101594A (en) * | 1975-03-05 | 1976-09-08 | Mitsubishi Chem Ind | Horiaminno bunriteiryoho |
| JPS60131457A (en) * | 1983-12-19 | 1985-07-13 | Shimadzu Corp | Device for analyzing bio-amine |
| KR20090027896A (en) * | 2007-09-13 | 2009-03-18 | 한국과학기술연구원 | Method for analysis of polyamines in urine or plasma using liquid chromatography/electronspray ionization-tandem mass spectrometry along with amine carbamylated derivatization |
| CN102788857A (en) * | 2012-08-03 | 2012-11-21 | 上海海洋大学 | Method for measuring biogenic amine in fresh chilled beef |
| CN103837635A (en) * | 2014-03-27 | 2014-06-04 | 中国热带农业科学院农产品加工研究所 | Method for determining content of biogenic amines in foods by adopting ultra-efficient bonded phase chromatography |
| CN104678003A (en) * | 2013-11-29 | 2015-06-03 | 沈阳药科大学 | Biomarker for evaluating liver cancer disease by using urine |
| CN106248855A (en) * | 2016-09-08 | 2016-12-21 | 河南中烟工业有限责任公司 | One assay method growing tobacco middle biogenic amine |
| CN106442840A (en) * | 2016-11-10 | 2017-02-22 | 河南中烟工业有限责任公司 | Method for measuring bioamine in main stream smoke of cigarettes |
-
2018
- 2018-04-24 CN CN201810412022.7A patent/CN108333275A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51101594A (en) * | 1975-03-05 | 1976-09-08 | Mitsubishi Chem Ind | Horiaminno bunriteiryoho |
| JPS60131457A (en) * | 1983-12-19 | 1985-07-13 | Shimadzu Corp | Device for analyzing bio-amine |
| KR20090027896A (en) * | 2007-09-13 | 2009-03-18 | 한국과학기술연구원 | Method for analysis of polyamines in urine or plasma using liquid chromatography/electronspray ionization-tandem mass spectrometry along with amine carbamylated derivatization |
| CN102788857A (en) * | 2012-08-03 | 2012-11-21 | 上海海洋大学 | Method for measuring biogenic amine in fresh chilled beef |
| CN104678003A (en) * | 2013-11-29 | 2015-06-03 | 沈阳药科大学 | Biomarker for evaluating liver cancer disease by using urine |
| CN103837635A (en) * | 2014-03-27 | 2014-06-04 | 中国热带农业科学院农产品加工研究所 | Method for determining content of biogenic amines in foods by adopting ultra-efficient bonded phase chromatography |
| CN106248855A (en) * | 2016-09-08 | 2016-12-21 | 河南中烟工业有限责任公司 | One assay method growing tobacco middle biogenic amine |
| CN106442840A (en) * | 2016-11-10 | 2017-02-22 | 河南中烟工业有限责任公司 | Method for measuring bioamine in main stream smoke of cigarettes |
Non-Patent Citations (8)
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Application publication date: 20180727 |