畜牧兽医学报 ›› 2008, Vol. 39 ›› Issue (12): 1772-1778.doi:

• 基础兽医 • 上一篇    下一篇

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

汪纪仓1,2,马素英1,3,王大菊1*,韩鹤友1,刘登才1   

  1. 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
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2008-12-24 发布日期:2008-12-24
  • 通讯作者: 王大菊

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

WANG Ji-cang1,2,MA Su-ying1,3,WANG Da-ju1*,HAN He-you1,LIU Deng-cai1   

  1. 1.National Reference Laboratory of Veterinary Drug Residues/MOA Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070,China; 2.College of Animal Science and Technology, Henan University of Science and Technology, Luoyang 471003,China; 3.Pharmacy College, Xinxiang Medical University, Xinxiang 453003, China
  • Received:1900-01-01 Revised:1900-01-01 Online:2008-12-24 Published:2008-12-24

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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3 mL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50 μL,50 ℃衍生60 min,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0.005~1.6 μg/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0.2 μg/kg,噻克硝唑为0.5 μg/kg,地美硝唑、甲硝唑和奥硝唑为1.0 μg/kg。空白肌肉组织样品中添加药物浓度在0.2~4.0 μg/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。

Abstract: 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 K2HPO4, followed by extracted with dichloromethane. The final solution was carefully evaporated just to dryness with a vacuum evaporator (water bath at 40 ℃). The remaining residues was dissolved with 3 mL ethyl acetate. The solution was transferred into a derivation tube, evaporated to dryness under a weak nitrogen stream and derivatised with a solution of 50 μL of BSA-50 μL of i-octane for 60 min at 50 ℃ to produce trimethylsilyl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, 0.5 μg/kg for SNZ, 1.0 μg/kg for DMZ, MNZ and ONZ. Recoveries of five nitroimidazoles in tissues spiked at 0.2-4.0 μg/kg were 74%-82%, the interday relative standard deviation was less than 13%. These results suggested that the developed method was a sensitive and accurate method for the determination of nitroimidazole residues in swine muscle.