動物源性食品中硝基咪唑殘留的HPLC檢測

論文編號:SW218  論文字數:9768,頁數:23

摘要：本研究以外標法為定量手段,建立禽肉、水產品、蜂蜜、蛋清中甲硝唑(Metronidazole, MTZ),地美硝唑(Dimetridazole, DMZ),奧硝唑（Omidazole, ONZ）,替硝唑(Tinidazole, TNZ),洛硝噠唑(Ronidazol,RNZ)殘留的高效液相色譜法。
 禽肉、水產品、蜂蜜中硝基咪唑類殘留的HPLC法：取肌肉組織經一系列樣品預處理,并在正己烷去脂后過MCX柱,經氨水甲醇溶液洗脫,色譜柱分離。流動相為醋酸氨緩沖液一乙腈(86:14,v：v ) ,320nm紫外檢測。結果顯示，測定禽肉組織中MTZ,DMZ,ONZ,TNZ,RNZ的最低檢測限和最低定量限1.0μg/kg，雞肉中回收率分別為90.8％,78.8％,75.1％,75.2％,83.2％；豬肉中的回收率分別為83.5％,76.1％,71.5%,75.2％,79.3％；大黃魚中的回收率分別為72.5%,75.0%,71.5%,72.7%,73.3%；蜂蜜中的回收率分別為82.6％,73.70％,76.23%,73.07％,80.6％。
 雞蛋中硝基咪唑類殘留的HPLC法：蛋黃,蛋清分別稱重，勻漿后精密稱取勻漿液10.0g，加異丙醇氯仿，超聲振蕩后離心，色譜柱分離。蛋清中的加標回收率分別為87.7%,71.2%,76.6%,73.7%,75.9%。
 本研究在國內首次建立硝基咪唑類藥物多組分殘留在肌肉、蜂蜜、雞蛋中的HPLC方法、靈敏度高，準確度和精密度均符合我國農業部獸藥殘留分析方法的要求，在國內同類研究中處于領先地位。
 關鍵詞 ： 硝基咪唑類藥物；高效液相色譜；動物源性食品

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