多壁碳纳米管固相萃取技术同时测定蜂蜜中多类兽药残留  

Simultaneous Determination of Multi-veterinary Drug Residues in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry and Multiwalled Carbon Nanotubes Cleaning

作　　者：曹慧[1,2] 陈小珍[1] 朱岩[2] 李祖光[3] 

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

出　　处：《高等学校化学学报》2013年第12期2710-2715,共6页Chemical Journal of Chinese Universities

基　　金：国家重大科学仪器设备开发专项(批准号:2012YQ09022903);浙江省科技厅钱江人才科技计划(批准号:2010R10044);浙江省质量技术监督系统科研计划(批准号:20110203)资助

摘　　要：采用多壁碳纳米管固相萃取-超高效液相色谱-串联质谱技术同时测定蜂蜜中的磺胺类、喹诺酮类、硝基咪唑类和四环素类等52种兽药残留.样品用Na2EDTA-Mcllvaine提取,经改性的多壁碳纳米管固相萃取小柱净化,通过Waters C18色谱柱分离,以乙腈和0.1%(体积分数)的甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测的质谱模式,以基质外标法进行定量分析.实验结果表明,52种兽药在相应的浓度范围内线性相关系数均大于0.99,该方法的定量限为1.5~7.5μg/kg.在7.5,25和50μg/kg 3个浓度添加水平下,各种兽药的回收率为67.3%~117.8%,相对标准偏差为1.9%~17.4%.结果表明,多壁碳纳米管固相萃取材料具有较好的净化效果,适用于蜂蜜中多类兽药残留的同时检测.A method for determining multi-veterinary drug residues in honey by ultra performance liquid chro- matography-tandem mass spectrometry（UPLC-MS/MS） and muhiwalled carbon nanotubes cleaning was estab- lished. This method enabled the comprehensive screening for 52 drugs including sulfonamides, quinolones, nitroimidazoles and tetracyclines. The samples were diluted by N%EDTA-Mellvaine solution （pH = 4 ） , the clean-up and proconcentration of the analytes were carried out by solid phase extraction cartridge packed with multi-walled carbon nanotubes（MWCNTs）. The target analytes were separated by Waters C18 column with gra- dient elution using acetonitrile and 0. 1% （volum fraction） formate in water as mobile phases. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reac- tion monitoring（MRM）. External standard method with matrix was used to determine the results. The correla- tion coefficient was greater than 0. 99 for each drugs. The limits of quantitation （LOQ） were 1.5--7.5 Ixg/kg. The mean recoveries at the three spiked levels of 7.5, 25, 50 I^g/kg were 67.3%--117.8%. The relative standard deviation（RSD） were 1.9%--17.4%. The results indicated that using multi-walled carbon nano- tubes as solid phase extraction adsorbent was efficient for the purification. The simplicity, sensitivity and good precision of the method made it be well suitable for determination of multi-veterinary drug residues in honey.

关 键 词：多壁碳纳米管 固相萃取 超高效液相色谱-串联质谱 残留 

分 类 号：O657.63[理学—分析化学]