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Method for testing cyclic dipeptide in white spirits

A cyclic dipeptide and liquor technology, applied in the field of chemical analysis, can solve the problems of false positives, difficult separation and low content of qualitative unknowns, and achieve the effects of good stability, high accuracy and good repeatability

Active Publication Date: 2014-12-10
WULIANGYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many kinds of cyclic dipeptides in liquor, and more than 20 kinds have been detected, but the content is usually very low, at the ug / L level or even lower, and a few are at the mg / L level, which is the detection zone for cyclic dipeptides in liquor come very difficult
[0004] According to related reports, the existing detection technology mainly uses LC-MS-MS, nuclear magnetic mass spectrometry and other instruments and equipment to detect, but for liquor, the relative content of cyclic dipeptide is low, and there are many flavor substances in the sample, which is difficult to detect. Separation, NMR mass spectrometry cannot be performed after purification as reported in the literature; LC-MS-MS is used for detection, because it is a low-resolution and high-sensitivity instrument, the mass accuracy is less than 2000ppm, and it is easy to cause false positives for qualitative unknowns. Standards must be used for control testing

Method used

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  • Method for testing cyclic dipeptide in white spirits
  • Method for testing cyclic dipeptide in white spirits
  • Method for testing cyclic dipeptide in white spirits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0101] a. Take 50mL of Luzhou-flavor liquor sample (52° Luzhou-flavor liquor), pass through the SPE C18 column, then elute with 50mL of methanol, and concentrate the eluate to 2mL at 40°C to obtain the sample to be tested;

[0102] b. Load the sample to be tested in step a to a liquid phase-mass spectrometer (LC-QTOF), and after mass spectrometry full-ion scanning, obtain a full-ion scanning chart (see figure 1 ), through all ion scanning peaks, it is preliminarily judged that there are ring (alanine-proline), ring (diaminobutyric acid), ring (leucine-alanine), ring (isoleucine-valine acid), ring (threonine-proline), ring (proline-phenylalanine), ring (phenylalanine-alanine), ring (leucine-isoleucine), Cyclic (valine-valine), cyclic (tyrosine-proline), cyclic (phenylalanine-valine), cyclic (proline-leucine), cyclic (diphenylalanine amino acid) exists;

[0103] Among them, liquid chromatography conditions: chromatographic column: Agilent Eclipse Plus C18 2.1*100mm 1.8-micron;...

Embodiment 2

[0113] a. Take 100mL of Fen-flavor liquor sample (53° Fen-flavor liquor), pass through the SPE C18 column, then elute with 50mL of methanol, and concentrate the eluate to 2mL at 30°C to obtain the sample to be tested;

[0114] b. Load the sample to be tested in step a to a liquid phase-mass spectrometer (LC-QTOF), and after mass spectrometry full-ion scanning, obtain a full-ion scanning diagram (see Figure 15 ), through all-ion scanning peaks, it is preliminarily determined that there are rings (alanine-proline), rings (phenylalanine-alanine), rings (leucine-isoleucine), rings (tyramine acid-proline), ring (phenylalanine-valine), ring (proline-leucine), ring (diphenylalanine) exist;

[0115] Among them, liquid chromatography conditions: chromatographic column: Agilent Eclipse Plus C18 2.1*100mm 1.8-micron; column temperature: 25°C; injection volume: 10uL; mobile phase: A: 0.1% formic acid aqueous solution, B: methanol; flow rate: 0.1 mL / min; Gradient elution method: 0-18min:...

Embodiment 3

[0125] a. Take 20 mL of Maotai-flavored liquor sample (53° Maotai-flavored liquor), pass it through the SPE C18 column, then elute with 50 mL of methanol, and concentrate the eluate to 2 mL at 60°C to obtain the sample to be tested;

[0126] b. Load the sample to be tested in step a to a liquid phase-mass spectrometer (LC-QTOF), and after mass spectrometry full-ion scanning, obtain a full-ion scanning chart (see Figure 23 ), through all ion scanning peaks, it is preliminarily judged that there are ring (alanine-proline), ring (diaminobutyric acid), ring (leucine-alanine), ring (isoleucine-valine acid), ring (threonine-proline), ring (proline-phenylalanine), ring (phenylalanine-alanine), ring (leucine-isoleucine), Cyclic (valine-valine), cyclic (tyrosine-proline), cyclic (phenylalanine-valine), cyclic (proline-leucine), cyclic (diphenylalanine acid);

[0127] Among them, liquid chromatography conditions: chromatographic column: Agilent Eclipse Plus C18 2.1*100mm 1.8-micron; ...

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Abstract

The invention relates to a method for testing cyclic dipeptide in white spirits. The method comprises the following steps: a, taking a white spirits sample, eluting with methanol after passing through an SPE-C18 column, and concentrating an eluent to 1 / 50-1 / 10 of the original volume of the white spirits sample at a temperature not higher than 60 DEG C to obtain a to-be-tested sample; b, loading the sample to be tested in step a to a liquid chromatograph-mass spectrometer, and after mass spectrum full-iron scanning, primarily obtaining possibly existing cyclic dipeptide through full-iron scanning peaks; c, then loading the sample to be tested in step a to the liquid chromatograph-mass spectrometer, and obtaining the characteristic ion peak of each possibly existing cyclic dipeptide after selected iron detection; d, further verifying whether the cyclic dipeptide obtained in step b exists in the white spirits or not according to the characteristic ion peak obtained in step c, and finally making a conclusion. The variety of the cyclic dipeptide in the white spirits sample can be accurately and rapidly tested by the method, and one more effective method is provided for the detection of the cyclic dipeptide in the white spirits.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for measuring cyclic dipeptides in liquor. Background technique [0002] Cyclic dipeptides, also known as 2,5-diketopiperazine derivatives, are found in humans, vertebrates, invertebrates, plants, fungi and bacteria It was found that because the cyclic dipeptide forms a stable six-membered ring structure with certain conformational constraints, there are two hydrogen bond donors and two hydrogen bond acceptors, and hydrogen bonds are one of the main ways in which drugs interact with receptors One, thus cyclic dipeptides are an important pharmacophore in medicinal chemistry. Many cyclic dipeptides have been found to have strong physiological activities, which have attracted widespread interest from organic chemists, biologists and pharmacologists. There are not many reports on cyclic dipeptides, and no reports about cyclic dipeptides in liquor have been found ...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 练顺才谢正敏廖勤俭李杨华彭智辅赵东乔宗伟安明哲王小琴
Owner WULIANGYE
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