High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor

A medium urethane, high performance liquid chromatography technology, applied in the field of analytical chemistry, can solve the problems of long time for chromatographic separation, complicated pretreatment methods, long time required, etc., and achieves short detection time, low cost, and accuracy. High performance and sensitivity

Active Publication Date: 2013-02-27
WULIANGYE
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Problems solved by technology

GC-MS analysis method is accurate and sensitive, but the pretreatment method is more complicated (currently, the pretreatment methods used for samples mainly include liquid-liquid extraction, solid-liquid extraction, solid-phase extraction, solid-phase microextraction, etc.), and the required time It is also longer; HPLC (high performance liquid chromatography) method needs to derivatize the sample (the EC content in distilled wine is low, and the ultraviolet detector cannot detect EC at the ppb level. Therefore, a relatively high-sensitivity fluorescence detector is required. However, EC itself does not produce fluorescence, so EC must be derivatized to bring a fluorescent group). Compared with GC-MS analysis, the pretreatment of HPLC method is relatively simple, but the sensitivity is low, and the chromatographic separation The time is also longer, and only rely on the retention time to qualify, the accuracy is poor

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  • High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor
  • High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor
  • High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor

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Embodiment Construction

[0019] The technical scheme of the present invention is a high-performance liquid chromatography-mass spectrometry detection method of urethane in distilled wine, comprising the following steps:

[0020] (1) Sample pretreatment: Measure a certain volume of distilled wine sample, remove the ethanol in the sample under reduced pressure with a rotary evaporator at 30~40°C, dilute to the original volume with distilled water, and filter;

[0021] (2) Detection: Take the processed distilled wine sample directly into LC-MS (liquid chromatography-mass spectrometry), select the protonated urethane molecular ion [M+H] + 90.055 is the quantitative ion for detection, and the content of urethane in the sample is calculated by the regression equation of the standard curve.

[0022] Further, the liquid chromatography conditions are as follows: the mobile phase is composed of A and B, wherein A is an aqueous solution containing 0.05-0.3% formic acid or acetic acid, B is acetonitrile or methan...

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Abstract

The invention belongs to the field of analytical chemistry, and relates to a high-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor. The invention aims to provide a method for quantitatively detecting ethyl carbamate in distilled liquor. The technical scheme is that the high-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor is characterized by comprising the following steps of: (1) pre-treating a sample; and (2) detecting. The method is simple to operate, the detection time is short, sensibility is high, and a result is precise.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a high-performance liquid chromatography-mass spectrometry detection method of urethane in distilled wine. Background technique [0002] Ethyl carbamate (EC), also known as urethane, was confirmed as a carcinogen as early as 1943. A large number of experimental data show that EC has a variety of metabolic modes in animals. Genotoxic and multi-site carcinogenic substances, which are classified as group 2B for human carcinogenic toxicity by the International Institute for Cancer Research. In 2007, the International Agency for Research on Cancer (IARC) re-evaluated EC and placed it in Group 2A, alongside lead and mercury, which means that EC may be carcinogenic to humans. Ethyl carbamate in beverage wine comes from its production and storage process. At present, only a few countries have formulated the limit standard for EC in beverage wine. [0003] The detection of ethyl carbam...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 唐桥陈林周韩玲练顺才李杨华廖勤俭
Owner WULIANGYE
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