同位素稀释-固相萃取-超高效液相色谱-串联质谱技术同时测定畜禽肉中四类兽药残留  

Determination of Four Species of Drugs in Meat by Solid Phase Extraction and UPLC-MS/MS with Isotopes Dilution

作　　者：曹慧[1,2] 陈小珍 朱岩[2] 李祖光[3] 汪丽娜[3] 张晓波[3] 

机构地区：[1]浙江省质量检测科学研究院,浙江杭州310013 [2]浙江大学化学系,浙江杭州310028 [3]浙江工业大学化学工程与材料学院,浙江杭州310014

出　　处：《质谱学报》2013年第4期202-214,共13页Journal of Chinese Mass Spectrometry Society

基　　金：浙江省科技厅分析测试科技计划项目(2011C37072);浙江省质量技术监督系统科研计划项目(20110203)资助

摘　　要：建立了畜禽肉中喹诺酮类、磺胺类、硝基咪唑类和青霉素类兽药的同位素稀释-固相萃取-超高效液相色谱-串联质谱分析方法。样品经V(Na2EDTA-Mcllvaine)∶V(乙腈)=7∶3的混合溶液提取,氮吹后经MCX小柱净化,Waters C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,内标法定量。在5～200μg/L质量浓度范围内,4类药物的相关系数均大于0.99,该方法的检出限在0.5～2.0μg/kg之间,定量限在2.0～6.5μg/kg之间。添加10、50、100μg/kg 3个浓度水平,4类药物的平均回收率在70.0%～130.9%之间,日内和日间相对标准偏差在1.03%～9.86%之间。将该技术应用于实际样品的测试,并采用液相色谱-离子阱-飞行时间质谱对阳性样品进行确证分析,通过多级质谱的精确质量数测定实现目标化合物的准确定性分析。该方法简单、快速、准确,适用于畜禽肉中多类兽药残留的快速检测和确证。The four species of drugs residues in meat were determined by solid phase extrac- tion and ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/ MS） with isotopes dilution. This method enabled the comprehensive screening for more than 50 drugs including quinolones, sulfonamides, nitroimidazoles and penicillin. The sam-ples were extracted with the mixed solution of Na2EDTA-Mcllvaine and acetonitrile, which volume ratio was 7 ： 3, a step for clean-up and proconcentration of the analytes by MCX solid phase extraction cartridge. The target analytes were separated by Waters C18 column with gradient elution using acetonitrile and 0.1% formate in water as mobile phases. The analytes were detected by positive electrospray ionization with multiple reaction monitoring （MRM）. Internal standard method was used to determine the results. In the linear range of 5--200 μg/L for each drugs, the correlation coefficient is greater than 0.99 for each antibi- otics. The limit of detection （LOD） is 0. 5--2. 0 μg/kg, and the limit of quantitation （LOQ） is 2.0--6.5 μg/kg. The mean recoveries at the three spiked levels of 10, 50,100 μg/kg are 70.0%--130.9%. The relative standard deviation （RSD） of intra-day and inter- day are 1.03 %--9.86 %. The proposed method was successfully applied to the analysis of real samples and trace of sulfamethazine and sulfadimoxine were detected in three samples. Identification of the positive samples is based on accurate mass measurement by liquid chro- matography-ion trap-time of flight tandem mass spectrometry. The method simplify, sensi- tivity and good precision, wich can be suitable for determination and confirmation of drugs residues in meat.

关 键 词：同位素稀释 固相萃取 超高效液相色谱-串联质谱(UPLC-MS MS) 兽药 残留 

分 类 号：O657.63[理学—分析化学]