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猪肉和禽肉组织中三种硝基咪唑残留荧光检测的高效薄层色谱法

High-performance thin-layer chromatographic method for the fluorescence detection of three nitroimidazole residues in pork and poultry tissue.

作者信息

Gaugain M, Abjean J P

机构信息

Centre National d'Etudes Vétérinaires et Alimentaires, Laboratoire des Médicaments Vétérinaires, Javené, France.

出版信息

J Chromatogr A. 1996 Jun 21;737(2):343-6. doi: 10.1016/0021-9673(96)00101-x.

DOI:10.1016/0021-9673(96)00101-x
PMID:8673259
Abstract

A high-performance thin-layer chromatographic method with fluorescence detection was developed for the qualitative determination of ronidazole, dimetridazole and their major metabolite, hydroxydimetridazole, in pork and poultry muscle. After extraction with dichloromethane and evaporation, the nitroimidazoles are redissolved in ammonium acetate buffer. The buffer phase is washed with hexane. The sample is cleaned-up by solid-phase extraction and the eluate evaporated. The final extract is resuspended in methanol and then spotted on an HPTLC plate. After multiple development with methanol and ethylacetate, the plate is dried, sprayed with pyridine and observed on an UV box (312 nm). The detection limits of this method are about 2 micrograms/kg for ronidazole, 5 micrograms/kg for dimetridazole and less than 5 micrograms/kg for hydroxydimetridazole. Validation was performed to levels of 10 micrograms/kg for dimetridazole, 5 micrograms/kg for ronidazole and 5 micrograms/kg for hydroxydimetridazole.

摘要

建立了一种带荧光检测的高效薄层色谱法,用于定性测定猪肉和禽肉中罗硝唑、地美硝唑及其主要代谢物羟基地美硝唑。用二氯甲烷萃取并蒸发后,将硝基咪唑重新溶解于醋酸铵缓冲液中。用己烷洗涤缓冲相。通过固相萃取对样品进行净化,然后将洗脱液蒸发。最终提取物重新悬浮于甲醇中,然后点样在高效薄层色谱板上。用甲醇和乙酸乙酯多次展开后,将板干燥,喷上吡啶,并在紫外灯箱(312 nm)上观察。该方法的检测限为:罗硝唑约2微克/千克,地美硝唑5微克/千克,羟基地美硝唑小于5微克/千克。针对地美硝唑10微克/千克、罗硝唑5微克/千克和羟基地美硝唑5微克/千克的水平进行了验证。

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