多壁碳纳米管净化-超高效液相色谱-串联质谱技术同时测定牛奶中青霉素类药物残留  

Determination of Penicillin Residues in Milk by Multiwalled Carbon Nanotubes Cleaning and UPLC-MS/MS

作　　者：曹慧[1,2] 陈小珍 朱岩[2] 李祖光[3] 祝颖 郑军科 

机构地区：[1]浙江省质量检测科学研究院,浙江杭州310030 [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》2015年第1期23-28,共6页Journal of Chinese Mass Spectrometry Society

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

摘　　要：研究了多壁碳纳米管净化-超高效液相色谱-串联质谱技术同时测定牛奶中的羟氨苄青霉素、青霉素V、氨苄青霉素、苯咪青霉素、甲氧苯青霉素、青霉素G、苯咪青霉素、邻氯青霉素、乙氧萘青霉素和双氯青霉素药物残留.样品用乙腈沉淀蛋白,提取液用磷酸缓冲液稀释后,经改性的多壁碳纳米管材料净化,通过Waters C18色谱柱分离,以乙腈和10 mmol/L乙酸铵（pH 4.5）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检测,内标法定量.10种青霉素药物在相应浓度范围内的线性相关系数均大于0.99,方法的定量限在0.1～10.0μg/kg之间.在低、中、高3个浓度添加水平下,10种青霉素药物的平均回收率为72.0％～110％,相对标准偏差在1.83％～9.33％之间.多壁碳纳米管材料具有较好的净化效果,该方法可以快速、准确地测定牛奶中的青霉素类药物残留.A method was established for determining penicillin residues in milk by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） and multiwalled carbon nanotubes cleaning. The samples were extracted by acetonitrile and diluted by phosphate buffer solution, a step for clean-up and proconcentration of the analytes by solid phase extraction cartridge packed with multi-walled carbon nanotubes （MWCNTs）. The target analytes were separated by Waters C18 column with gradient elution using acetonitrile and 10 mmol/L ammonium acetate （pH 4.5） as mobile phases. The analytes were detected by tandem quadrupole mass spectrometry after positive elec- trospray ionization by multiple reaction monitoring （MRM）. Internal standard method with matrix was used to determine the results. The correlation coefficient is greater than 0.99 for each drugs. The limits of quantitation （LOQ） are 0.1-10.0 μg/kg. The mean recoveries at the three spiked levels are 72.0%-110%. The relative standard deviations （RSDs） are 1.83%-9. 33%. The results indicated that using multi-wailed carbon nano- tubes as solid phase extraction adsorbent is efficient for the purification. The simplicity, sensitivity and good precision of the method made it is well suitable for determination of penicillin residues in milk.

关 键 词：多壁碳纳米管 固相萃取 超高效液相色谱-串联质谱(UPLC-MS/MS) 牛奶 青霉素 

分 类 号：O657.63[理学—分析化学]