CN108872414A - A kind of method that LC-MS/MS measures the cadaverine in soy sauce - Google Patents
A kind of method that LC-MS/MS measures the cadaverine in soy sauce Download PDFInfo
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- CN108872414A CN108872414A CN201810412011.9A CN201810412011A CN108872414A CN 108872414 A CN108872414 A CN 108872414A CN 201810412011 A CN201810412011 A CN 201810412011A CN 108872414 A CN108872414 A CN 108872414A
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- soy sauce
- cadaverine
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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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Soy Sauces And Products Related Thereto (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses the methods of the cadaverine in a kind of LC-MS/MS measurement soy sauce, are monitored using reaction of high order, and quantitative with ion pair 103.2=> 86.1, ion pair 103.2=> 69.1 is 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 cadaverine detection method in a kind of soy sauce.
Background technique
Cadaverine is one kind of biogenic amine, and cadaverine is the product of lysine decarboxylation under the action of decarboxylase.In sauce fermentation
In the process, there is a large amount of lysine, some cadaverines can be generated in the effect of microorganism, soy sauce.Therefore, the corpse in soy sauce is detected
Amine is particularly significant.Currently used method is to be detected after cadaverine derivatization with liquid phase, but this method is time-consuming longer.The present invention is logical
After diluting soy sample, using the cadaverine content in reaction of high order monitoring (MRM) analysis soy sauce.
Summary of the invention
It is an object of the present invention to the problem of overcoming the complex pretreatment of the prior art, corpse in a kind of soy sauce is provided
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 of gas temperature, flow velocity 8L/min, capillary voltage 4000V,
Positive ion mode.Fragmentation voltage 65, fragmentation voltage 9, acceleration voltage 4, quota ion pair 103.2=> 86.1；Fragmentation voltage 65,
Fragmentation voltage 17, acceleration voltage 4, qualitative ion pair 103.2=> 69.1.
3 weigh a certain amount of tryptamines standard items, prepare the standard solution of certain gradient, carry out LC-MS/MS analysis.
4. soy sample dilutes 400-1000 times, direct injection analysis.
5. integral retention time is 1.037min peak area, calibration curve is determined.The retention time for bringing sample into is
1.037min peak area calculates concentration × extension rate, i.e. the tryptamines content of soy sauce.
Detailed description of the invention
Attached drawing is the matched curve in embodiment 1.
Specific embodiment：
Below by specific embodiment, technical scheme is described further：
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 column.
2 Mass Spectrometry Conditions：Using electric spray ion source, 300 DEG C of gas temperature, flow velocity 8L/min, capillary voltage 4000V,
Positive ion mode.Fragmentation voltage 65, collision energy 9, acceleration voltage 4, quota ion pair 103.2=> 86.1；Fragmentation voltage 65,
Collision energy 17, acceleration voltage 4, qualitative ion pair 103.2=> 69.1.
3 weigh a certain amount of putrescine standard items, prepare 6.9 μ g/L, 34.6 μ g/L, 173.2 μ g/L, and the standard of 86.6 μ g/L is molten
Liquid, sample volume are 5 μ L, carry out LC-MS/MS analysis.Integral retention time is 1.037min peak area, obtains calibration curve y=
703.94x+12569, R2=0.997 wherein y be peak area, x is Putrescine concentration.
4. soy sample dilutes 1000 times, sample volume is 5 μ L.
5. the retention time for bringing sample into is 1.037min peak area 22150, according to calibration curve, obtaining x is 18.6 μ g/L,
Calculate concentration × extension rate, i.e., tryptamines content 18.6mg/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 83%-96%.
Claims (1)
1. a kind of method of cadaverine in LC-MS/MS measurement soy sauce, it is characterised in that：Using the diluted method of soy sauce, quota ion
To 103.2=> 86.1；Qualitative ion pair 103.2=> 69.1.Gradient concentration is done with cadaverine standard items, carries out the analysis of liquid matter,
Matched curve is obtained, the concentration of cadaverine in soy sauce is calculated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810412011.9A CN108872414A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the cadaverine in soy sauce |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810412011.9A CN108872414A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the cadaverine in soy sauce |
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| CN108872414A true CN108872414A (en) | 2018-11-23 |
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| CN201810412011.9A Pending CN108872414A (en) | 2018-04-24 | 2018-04-24 | A kind of method that LC-MS/MS measures the cadaverine in soy sauce |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6479654A (en) * | 1987-09-22 | 1989-03-24 | Shimadzu Corp | Polyamine analysis |
| WO2011034539A1 (en) * | 2009-09-18 | 2011-03-24 | The Regents Of The University Of California | Methods for detecting autodigestion |
| CN102788857A (en) * | 2012-08-03 | 2012-11-21 | 上海海洋大学 | Method for measuring biogenic amine in fresh chilled beef |
| CN102914606A (en) * | 2012-10-20 | 2013-02-06 | 江南大学 | Qualitative and quantitative method for various biogenic amines in white wine |
| CN105866316A (en) * | 2016-06-24 | 2016-08-17 | 曲阜师范大学 | Analysis method for simultaneous detection of amino acids and biogenic amines in foods |
| CN107782834A (en) * | 2016-08-25 | 2018-03-09 | 中国科学院大连化学物理研究所 | A kind of rapid analysis method for being directed to biogenic amine in fish |
-
2018
- 2018-04-24 CN CN201810412011.9A patent/CN108872414A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6479654A (en) * | 1987-09-22 | 1989-03-24 | Shimadzu Corp | Polyamine analysis |
| WO2011034539A1 (en) * | 2009-09-18 | 2011-03-24 | The Regents Of The University Of California | Methods for detecting autodigestion |
| CN102788857A (en) * | 2012-08-03 | 2012-11-21 | 上海海洋大学 | Method for measuring biogenic amine in fresh chilled beef |
| CN102914606A (en) * | 2012-10-20 | 2013-02-06 | 江南大学 | Qualitative and quantitative method for various biogenic amines in white wine |
| CN105866316A (en) * | 2016-06-24 | 2016-08-17 | 曲阜师范大学 | Analysis method for simultaneous detection of amino acids and biogenic amines in foods |
| CN107782834A (en) * | 2016-08-25 | 2018-03-09 | 中国科学院大连化学物理研究所 | A kind of rapid analysis method for being directed to biogenic amine in fish |
Non-Patent Citations (4)
| Title |
|---|
| LISA M. SWANN等: "Determination of amino acids and amines in mammalian decomposition fluid by direct injection liquid chromatography-electrospray ionisation-tandem mass spectrometry", 《ANALYTICAL METHODS》 * |
| SANGHEE LEE等: "Determination of Biogenic Amines in Cheonggukjang Using Ultra High Pressure Liquid Chromatography Coupled with Mass Spectrometry", 《FOOD SCIENCE AND BIOTECHNOLOGY》 * |
| 周朝晖 等: "QuEChERS-UPLC-MS/MS法测定酱油中8种生物胺", 《现代食品科技》 * |
| 许禄 等: "黄酒中生物胺的HPLC-MS/MS测定", 《山东农业大学学报（自然科学版）》 * |
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Application publication date: 20181123 |