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

doi:10.7503/cjcu20130764

高等学校化学学报 ›› 2013, Vol. 34 ›› Issue (12): 2710.doi: 10.7503/cjcu20130764

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

曹慧^1,2, 陈小珍¹, 朱岩², 李祖光³

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

收稿日期:2013-08-06 出版日期:2013-12-10 发布日期:2013-10-23
作者简介:曹慧，女，博士，高级工程师，主要从事色谱-质谱联用方面的研究. E-mail：ch_zj_cn@163.com
基金资助:
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）和浙江省质量技术监督系统科研计划（批准号：20110203）资助.

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

CAO Hui^1,2, CHEN Xiao-Zhen¹, ZHU Yan², LI Zu-Guang³

1. Zhejiang Institute of Quality Inspection Science, Zhejiang Food Safety Key Laboratory, Hangzhou 310013, China;
2. Department of Chemistry, Zhejiang University, Hangzhou 310028, China;
3. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China

Received:2013-08-06 Online:2013-12-10 Published:2013-10-23

摘要/Abstract

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 ~7.5 μg/kg. 在7.5，25和50 μg/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.

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

Abstract:

A method for determining multi-veterinary drug residues in honey by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) and multiwalled carbon nanotubes cleaning was established. This method enabled the comprehensive screening for 52 drugs including sulfonamides, quinolones, nitroimidazoles and tetracyclines. The samples were diluted by Na₂EDTA-Mcllvaine 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 gradient 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 reaction monitoring(MRM). External standard method with matrix was used to determine the results. The correlation coefficient was greater than 0.99 for each drugs. The limits of quantitation(LOQ) were 1.5—7.5 μg/kg. The mean recoveries at the three spiked levels of 7.5, 25, 50 μg/kg were 67.3%—117.8%. The relative standard deviation(RSD) were 1.9%—17.4%. The results indicated that using multi-walled carbon nanotubes 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.

Key words: Multiwalled carbon nanotubes(MWCNTs), Solid phase extraction, Ultra performance liquid chromatography-tandem mass spectrometry, Residue

中图分类号:

O657.63

TrendMD:

曹慧, 陈小珍, 朱岩, 李祖光. 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. 高等学校化学学报, 2013, 34(12): 2710.

CAO Hui, CHEN Xiao-Zhen, ZHU Yan, LI Zu-Guang. Simultaneous Determination of Multi-veterinary Drug Residues in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry and Multiwalled Carbon Nanotubes Cleaning. Chem. J. Chinese Universities, 2013, 34(12): 2710.

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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

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