A liquid chromatography-tandem mass spectrometry method for the determination of chloramphenicol residues in milk powder

Abstract

The invention discloses a liquid chromatogram-mass spectrum / mass spectrum (LC-MS / MS) determination method for chloramphenicol residue amount in milk powder. Milk powder is rich in protein, fat, carbohydrate, and the like, and therefore a serious emulsification phenomenon is produced in direct extraction and determination of the lipophilic chloramphenicol by using ethyl acetate, and the chloramphenicol cannot be extracted. The method provided by the invention comprises steps of dissolving a sample with a sodium chloride solution, adding acetonitrile to precipitate the protein, extracting with ethyl acetate, blow-drying the extract by using nitrogen, redissolving by using an acetonitrile aqueous solution, adding hexane for purification to remove the fat, determining by using LC-MS / MS, and quantifying by using an internal standard method. The method provided by the invention has advantages of simple operation steps, high extraction efficiency, reasonable purification technology, low cost and good effects. The method detection limit is 0.1 [mu]g / kg, reaching an advanced level of sample chloramphenicol residue amount determination method at home and abroad.

Description

technical field [0001] The invention belongs to the field of ultra-trace chemical analysis, in particular to a liquid chromatography-tandem mass spectrometry method for determining the residual amount of chloramphenicol in milk powder samples with complex components. Background technique [0002] Chloramphenicol is one of the broad-spectrum antibiotics, which was commonly used in the treatment of various infectious diseases in animals in the past. Chloramphenicol has serious toxic and side effects. Residues in animal tissues not only cause direct harm to animals and humans, but also induce drug resistance of pathogenic bacteria, posing a huge threat to human health. [0003] At present, there are many detection standards for chloramphenicol residues, mainly focusing on aquatic products and other animal-derived foods. After searching, no detection standards for chloramphenicol residues in milk powder have been found, and only a small amount of detection methods for chloramphe...

AI Technical Summary

Problems solved by technology

[0004] The purpose of the embodiments of the present invention is to provide a liquid chromatography-tandem mass spectrometry method for the determination of chloramphenicol residues in milk powder, aiming at solving the problem of milk powder samples with no applicable detection method and complex components for the chloramphenicol residue in milk powder samples The problem of extraction and purification technology provides a simple and easy-to-operate extraction, purification, instrument determination steps suitable for the residual amount of chloramphenicol in milk powder, and a detection method with sufficient instrument conditions

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