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Method for detecting content of ethyl carbamate in soybean-flavor Baijiu

A technology of medium urethane and urethane, applied in the field of analytical chemistry, can solve problems such as poor accuracy and quantification, large loss of reagents, cumbersome pretreatment, etc., to save detection time, improve recovery rate, and pretreatment The effect of simple processing

Inactive Publication Date: 2016-10-26
GUANGDONG SHIWAN WINE GRP CO LTD
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Problems solved by technology

Compared with the external standard method of gas chromatography-mass spectrometry, the internal standard method of gas chromatography-mass spectrometry has improved the accuracy and stability of the method. However, gas chromatography-mass spectrometry has problems such as cumbersome pretreatment, long time-consuming, and large loss of reagents.
Liquid chromatography fluorescence method is simple and fast, but the accuracy and quantification are not good

Method used

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  • Method for detecting content of ethyl carbamate in soybean-flavor Baijiu
  • Method for detecting content of ethyl carbamate in soybean-flavor Baijiu
  • Method for detecting content of ethyl carbamate in soybean-flavor Baijiu

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Embodiment Construction

[0050] 1. Preparation of standard solution

[0051] Urethane stock solution (100 μg / mL): Accurately weigh 10 mg of urethane standard, dissolve in methanol, dilute to 100 mL, and store in a refrigerator at 4°C.

[0052] Butyl carbamate stock solution (100 μg / mL): Accurately weigh 10 mg of butyl carbamate standard, dissolve in methanol, dilute to 100 mL, and store in a refrigerator at 4°C.

[0053] Urethane intermediate solution (1000μg / L): Accurately pipette 1mL of urethane stock solution (100μg / mL), dilute to 100mL with methanol-water (1:9v / v) solution, and store in a refrigerator at 4°C.

[0054] Butyl carbamate intermediate solution (1000 μg / L): Accurately pipette 1 mL of butyl carbamate stock solution (100 μg / mL), dilute to 100 mL with methanol-water (1:9 v / v) solution, and store in a refrigerator at 4 °C.

[0055] Standard curve working solution: respectively draw 10 μL, 20 μL, 50 μL, 100 μL, 200 μL, and 500 μL of urethane intermediate solution (1000 μg / L) into six 10 mL ...

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Abstract

The invention discloses a method for detecting a content of ethyl carbamate in soybean-flavor Baijiu. The method comprises a sample preprocessing step and an LC-MS detection step, wherein in the sample preprocessing step, a sample is prepared by the following steps: sucking 1mL of sample, placing the sample into a 10mL bottle, adding 100 microliters of 1000 microgram / L ethyl carbamate inner marker, ensuring the volume to 10mL by using distilled water, uniformly mixing, filtering by a 0.22 micrometer organic filter membrane, and performing the LC-MS determination for filtrate; and in the LC-MS detection step, detecting the content of the ethyl carbamate in the filtrate by using a liquid chromatography-mass spectrometer. In the detection method, the sample is directly loaded onto a machine after being diluted by using the distilled water and then filtered by the microporous filter membrane, so that the preprocessing process of the sample is simplified, and the recovery rate of the method and the stability of a detection result are improved.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, relates to the analysis and detection of trace components in liquor, and specifically discloses a liquid chromatography-mass spectrometry detection method for ethyl carbamate in soy-flavored liquor. The detection method can save the organic solution in the sample pretreatment process The use of simplifies the pretreatment process of samples and improves the accuracy and sensitivity of detection results. Background technique [0002] Ethyl carbamate (abbreviated as EC) is a natural substance produced during food fermentation and storage, and is widely found in fermented wine, yogurt, soy sauce and other fermented products. Urethane is genotoxic and carcinogenic. In 2007, the International Agency for Research on Cancer (IARC) officially classified EC as a Class 2A carcinogen (ie, a possible human carcinogen). [0003] At present, the existing standard methods for EC detection at home and abroad...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/027G01N2030/884
Inventor 郭波郑扬韵孙心恒
Owner GUANGDONG SHIWAN WINE GRP CO LTD
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