摘要
【目的】建立猪肌肉、脂肪、肝脏和肾脏中羟基地美硝唑、洛硝唑、甲硝唑、替硝唑、地美硝唑和奥硝唑残留的高效液相色谱(HPLC)测定法。【方法】样品中硝基咪唑类药物用二氯甲烷萃取,盐酸反萃取。盐酸溶液用K2HPO4碱化,再用二氯甲烷反萃取,萃取液于40℃水浴中旋转真空蒸干。残余物用流动相0.5ml溶解,进样分析。色谱柱为Hypersil ODS2,紫外检测器,检测波长320nm。以甲醇﹕水(14﹕86,V﹕V)为流动相,进样量20μl。【结果】6种药物标准液浓度在0.005～2.0μg·ml-1时,与响应值呈良好线性关系,相关系数均>0.999。羟基地美硝唑、洛硝唑和甲硝唑在肌肉和脂肪组织中检测限为0.5μg·kg-1,在肝脏和肾脏中为1.0μg·kg-1;替硝唑、地美硝唑和奥硝唑在肌肉、脂肪、肝脏和肾脏中均为1.0μg·kg-1。空白样品添加药物浓度为0.5～4.0μg·kg-1时,6种药物的回收率为60%～83%,日间变异系数均<15%。【结论】该方法能灵敏、准确的检测猪组织中硝基咪唑类药物。
[Objective] A high-performance liquid chromatographic （HPLC） method is described for the determination of HMMNI, RNZ, MNZ, TNZ, DMZ and ONZ residues in swine tissues. [Method] The nitroimidazole residues were extracted with dichloromethane, followed by reextraction with hydrochloric acid. The acid extract was made basic with K2HPO4, followed by extraction with dichloromethane. The final solution was carefully evaporated just to dryness with a vacuum evaporator （water bath at 40℃）. The residues were redissolved in 0.5 ml mobile phase. Detection wavelength was set at 320 nm and the injection volume was 20 μl. The mobile phase was methanol and water （16 ： 84, V ： V）. [ Result ] The linear regression curves yielded correlation coefficients of over 0.999 of the six nitroimidazoles. The limits of detection were 0.5 μg·kg^-1 for HMMNI, RNZ, MNZ and 1.0 μg·kg^-1 for TNZ, DMZ, ONZ in muscle and fat, 1.0 μg·kg^-1 for HMMNI, RNZ, MNZ, TNZ, DMZ and ONZ in liver and kidney. The control samples were all spiked with nitroimidazoles at levels of 0.5-4.0 μg·kg^-1. The mean recoveries of nitroimidazoles were 60%-83%, the inter-day relative standard deviation was less than 15%. [Conclusion] It is concluded that it is a sensitive and accurate method for determination of nitroimidazole residues in swine tissues.
出处
《中国农业科学》
CAS
CSCD
北大核心
2008年第10期3318-3325,共8页
Scientia Agricultura Sinica
基金
农业部兽药残留专项基金资助项目(2003,76号)
关键词
硝基咪唑类药物
猪
组织
残留
高效液相色谱法
Nitroimidazole
Swine
Tissue
Residues
High-performance liquid chromatography
