动物源性食品中硝基咪唑残留的HPLC检测

论文编号:SW218  论文字数:9768,页数:23

摘要：本研究以外标法为定量手段,建立禽肉、水产品、蜂蜜、蛋清中甲硝唑(Metronidazole, MTZ),地美硝唑(Dimetridazole, DMZ),奥硝唑（Omidazole, ONZ）,替硝唑(Tinidazole, TNZ),洛硝哒唑(Ronidazol,RNZ)残留的高效液相色谱法。
 禽肉、水产品、蜂蜜中硝基咪唑类残留的HPLC法：取肌肉组织经一系列样品预处理,并在正己烷去脂后过MCX柱,经氨水甲醇溶液洗脱,色谱柱分离。流动相为醋酸氨缓冲液一乙腈(86:14,v：v ) ,320nm紫外检测。结果显示，测定禽肉组织中MTZ,DMZ,ONZ,TNZ,RNZ的最低检测限和最低定量限1.0μg/kg，鸡肉中回收率分别为90.8％,78.8％,75.1％,75.2％,83.2％；猪肉中的回收率分别为83.5％,76.1％,71.5%,75.2％,79.3％；大黄鱼中的回收率分别为72.5%,75.0%,71.5%,72.7%,73.3%；蜂蜜中的回收率分别为82.6％,73.70％,76.23%,73.07％,80.6％。
 鸡蛋中硝基咪唑类残留的HPLC法：蛋黄,蛋清分别称重，匀浆后精密称取匀浆液10.0g，加异丙醇氯仿，超声振荡后离心，色谱柱分离。蛋清中的加标回收率分别为87.7%,71.2%,76.6%,73.7%,75.9%。
 本研究在国内首次建立硝基咪唑类药物多组分残留在肌肉、蜂蜜、鸡蛋中的HPLC方法、灵敏度高，准确度和精密度均符合我国农业部兽药残留分析方法的要求，在国内同类研究中处于领先地位。
 关键词 ： 硝基咪唑类药物；高效液相色谱；动物源性食品

Abstract：This paper established the reverse phase high performance liquid chromatogra-
phic methods of nitroimidazoles residues detection in animals edible tissues, marine lives, bee products and egg albumen by the means of extemal standard.
 The HPLC methods of Nitroimidazoles in animals edible tissues: After an initial extraction with ethyl acetate and evaporation in sequence, the sample was resolved in hydrochloric acid. Hexane was used in the liquid-liquid extraction to remove fat. A MCX solid phase separation was performed and used ammonia and methanol as eluates. Then HPLC analysis carried out as follows: Detecting wavelengh was at 320nm and mobile phase was acetate buffer solution and acetonitrile(86:14,v/v). The limits of detection and quantification for nitroimidazoles were 1.0μg/kg. Recovery ratios of MTZ, DMZ, ONZ, TNZ, RNZ in chicken were 90.8％, 78.8％, 75.1％, 75.2％, 83.2％; in pork tissue were 83.5％,76.1％,71.5%,75.2％,79.3％; in aquatic products were 72.5%, 75.0%,71.5%,72.7%,73.3%; in bee product were 82.6％,73.7％, 76.2%, 73.1％, 80.6％.
 The HPLC methods of Nitroimidazoles in eggs albumen: eggs albumen(10g) was put in a centrifuge tube. Isopropanol and chloroform were added, the tissue was dispersed by vortex-mixing and placed in an ultrasonic bath. Finally, after centrifugation the hexane fraction was discarded. The recovery ratios were 87.7%,71.2%,76.6%,73.7%,75.9%.
 The results showed that this method was enough sensitive, accurate and precise to deteminate the nitroimidazoles residues and can be applied to determinate nitroimidazoles residues in animal edible tissue.
 Key words：Nitroimidazoles; HPLC; animals edible product
 

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