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Detection method of various biological toxins in fermented wine

A technology for biological toxins and detection methods, applied in the field of chemical detection, can solve the problems of ion source pollution, low recovery rate, high cost of chromatography columns and mass spectrometry systems, and achieve the effects of saving detection costs, high accuracy, and simple sample processing.

Inactive Publication Date: 2016-08-24
中华人民共和国苏州出入境检验检疫局
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, immunoaffinity columns or other solid-phase extraction columns are usually used to enrich and purify the target, or directly inject samples, and use liquid chromatography or liquid chromatography-mass spectrometry for detection, but high cost, low efficiency, low recovery and Some target analytes have obvious matrix enhancement or weakening effects due to direct injection, and the ion source contamination of the chromatographic column and mass spectrometry system

Method used

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  • Detection method of various biological toxins in fermented wine
  • Detection method of various biological toxins in fermented wine
  • Detection method of various biological toxins in fermented wine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Multiple biotoxin residue detection in rice wine of embodiment 1

[0034] (1) Preparation of standard solution: Weigh 10 mg of standard samples of ochratoxin, aflatoxin, citrinin, mantletoxin, and patulin respectively, and dissolve each standard sample with acetonitrile as solvent and constant volume Obtain the mother solution of the standard solution, and the concentration of the mother solution is 1mg / mL, and then use the acetonitrile water (3+2) solution to dilute the mother solution into a certain concentration of the standard solution as required, and store it at -18°C for future use;

[0035] (2) Sample treatment: Take 5ml of wine sample in a 50ml centrifuge tube, add 10ml of chloroform, vortex and oscillate at a high speed on a vortex shaker for 2 minutes, after standing for stratification, transfer all the lower organic phase to a 10ml centrifuge tube In the tube, blow it dry with nitrogen in a water bath below 40°C, add 1ml of acetonitrile water (3+2) solution ...

Embodiment 2

[0062] Multiple toxin residue detection in wine of embodiment 2

[0063] Sample processing: take the wine sample and process it according to the same processing method as in Example 1;

[0064] Determination: Get the test solution prepared in this embodiment and inject samples for analysis and determination, and the chromatographic mass spectrometry conditions are completely consistent with those in Example 1, and the spectrogram of the test solution obtained is as follows: Figure 3A / 3B, and the residual amount of ochratoxin A, aflatoxin B1, aflatoxin M1, citrinin, mantis, and patulin in the liquid to be tested is obtained through quantitative calculation of the workstation software (see Table c ).

[0065] Multiple toxin residues (ng / mL) in table c example 2 samples

[0066] Target

Embodiment 3

[0067] Multiple toxin residue detection in cider of embodiment 3

[0068] Sample treatment: take the cider sample and process it according to the same treatment method as in Example 1;

[0069] Determination: Get the test solution prepared in this embodiment and inject samples for analysis and determination, and the chromatographic mass spectrometry conditions are completely consistent with those in Example 1, and the spectrogram of the test solution obtained is as follows: Figure 4A / 4B, and through the quantitative calculation of the workstation software, the residual amounts of ochratoxin A, aflatoxin B1, aflatoxin M1, citrinin, mantis, and patulin in the liquid to be tested are obtained (see Table d ).

[0070] Multiple toxin residues (ng / mL) in table d example 3 samples

[0071] Target

[0072] The method of the present invention can simultaneously measure the content of various biological toxins in the sample in a relatively short period of time, and the sam...

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Abstract

The invention provides a method for measuring various biological toxins in fermented wine by liquid chromatography-mass spectrometry. It only needs to extract the sample through simple liquid-liquid distribution and transfer the extract to dissolve to obtain the liquid to be tested, that is, the sample processing is simple, The ESI source is used as the ion source, the Inertsil C8 chromatographic column is used, and the gradient elution separation is carried out at a flow rate of 0.25mL / min. The mobile phase is 5mmol / L ammonium acetate aqueous solution A and acetonitrile B, which meets the collection of positive and negative ions The mode works at the same time, and can simultaneously measure the content of multiple biological toxins in the sample in a short period of time. It avoids the high cost, low efficiency, low recovery rate and other problems caused by using immunoaffinity columns or other solid-phase extraction columns to enrich and purify target substances in the prior art, or some target analytes are ineffective due to direct injection. Significant matrix enhancement or weakening effects, as well as contamination of the chromatographic column and mass spectrometer system ion source caused by direct injection, thereby reducing the corresponding maintenance costs.

Description

technical field [0001] The invention relates to chemical detection, in particular to a method for determining multiple biological toxins in fermented wine. Background technique [0002] Fermented wine is a beverage wine with an alcohol content of less than 24%, which is made from grains, fruits, milk, etc., mainly through yeast fermentation and other processes. It mainly includes beer, wine, fruit wine and rice wine. [0003] More than 300 mycotoxins with very different structures are known, some of the main mycotoxins are: aflatoxin (Aflatoxin), ergot alkaloids, ochratoxin A, 3-nitropropionic acid, patulin , Fusarium toxin (a zearalenone; b trichothecene compounds such as: such as T2 toxin), citrinin, chrysogreen penicillin, vertigomycin, these toxins are harmful to the liver, kidney, lung, heart, brain, etc. There are varying degrees of damage to vital organs of the human body, causing teratogenic and carcinogenic hazards. During the production process of fermented wine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 陈军谢鑫陟樊继鹏徐罕琦徐振东
Owner 中华人民共和国苏州出入境检验检疫局