气相色谱-离子阱串联质谱法同时测定猪肌肉中硝基咪唑类药物残留量  

Simultaneous Determination of Nitroimidazole Residues in Swine Meat by Gas Chromatography-Ion Trap Tandem Mass Spectrometry

作　　者：汪纪仓[1,2] 马素英[1,3] 王大菊[1] 韩鹤友[1] 刘登才[1] 

机构地区：[1]华中农业大学国家兽药残留基准实验室／农业部食品安全评价重点开放实验室,武汉430070 [2]河南科技大学动物科技学院,洛阳471003 [3]新乡医学院药学院,新乡453003

出　　处：《畜牧兽医学报》2008年第12期1772-1778,共7页ACTA VETERINARIA ET ZOOTECHNICA SINICA

基　　金：农业部兽药残留专项农办牧[2003]76号

摘　　要：旨在建立测定猪肌肉中地美硝唑、洛硝唑、噻克硝唑、甲硝唑和奥硝唑等硝基咪唑类药物残留的气相色谱一离子阱串联质谱测定法。样品用二氯甲烷提取，盐酸反萃取。盐酸萃取液用磷酸氢二钾碱化，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3mL乙酸乙酯溶解，于40℃水浴氮气吹干，加入N，O-双（三甲基硅烷基）乙酰胺和异辛烷各50pL，50℃衍生60min，进样分析，GC—MS／MS检测，外标法定量。结果表明，5种药物标准液浓度在0．005～1．6μg／mL时，与响应值呈良好线性关系，相关系数均大于0．998。洛硝唑的检测限可达0．2μg／kg，噻克硝唑为O．5μg／kg，地美硝唑、甲硝唑和奥硝唑为1．0μg／kg。空白肌肉组织样品中添加药物浓度在0．2～4．0μg／kg时，5种药物的回收率为74％～82％，日间变异系数均小于13％。表明所建立方法灵敏、准确，可用于检测猪肌肉中硝基咪唑类药物残留。A gas chromatography-ion trap tandem mass spectrometry method was developed for the determination of DMZ, RNZ, SNZ, MNZ and ONZ residues in swine muscle. The nitroimidazole residues were extracted with dichloromethane, followed by reextracted with hydrochloric acid. The acid extract was made basified with K2 HPO4 , followed by extracted with dichlorometh-ane. The final sol bath at 40℃）. T transferred into a utlon he re deriv vatised with a solution was carefully evaporated just to dryness with a vacuum evaporator （water maining residues was dissolved with 3 mL ethyl acetate. The solution was ation tube, evaporated to dryness under a weak nitrogen stream and deriof 50μL of BSA 50μL of i-octane for 60 min at 50 ℃ to produce trimeth-ylsilyl-derivatives （TMS-derivatives）. The resulting mixture was directly injected into the GC- MS/MS system. It was shown that the calibration curves were linear with a correlation coefficients （r） over 0. 998 in range of 0. 005-1.6 μg/mL. The limits of detection were 0.2 μg/kg for RNZ, 0. azoles in tion was accurate 5 μg/kg for SNZ, 1.0 μg/kg for DMZ, MNZ and ONZ. Recoveries of five nitroimidtissues spiked at 0. 2-4.0 μg/kg were 74%-82%, the inter-day relative standard devia- less than 13%. These results suggested that the developed method was a sensitive and method for the determination of nitroimidazole residues in swine muscle.

关 键 词：硝基咪唑类药物 猪 肌肉 残留 气相色谱离子阱串联质谱法 

分 类 号：S859.84[农业科学—临床兽医学]