超高效液相色谱-串联质谱法测定10种食品中的阿维菌素类药物残留

食品科学 ›› 2012, Vol. 33 ›› Issue (18): 226-231.

超高效液相色谱-串联质谱法测定10种食品中的阿维菌素类药物残留

张文娟1，连庚寅2，郭晓喜2，杨小兰1，宋欢2,*

1.山西大学生命科学学院 2.山西出入境检验检疫局

收稿日期:2011-07-07 修回日期:2012-07-22 出版日期:2012-09-25 发布日期:2012-09-07
通讯作者: 宋欢 E-mail:huanle_song@163.com
基金资助:
国家质检总局科研项目

Determination of Avemectin Residues in 10 Foods by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Received:2011-07-07 Revised:2012-07-22 Online:2012-09-25 Published:2012-09-07

摘要/Abstract

摘要： 建立以超高效液相色谱-电喷雾串联质谱同时检测10种食品中的阿维菌素类药物(包括阿维菌素、伊维菌素、多拉菌素、依普菌素、莫西丁克和塞拉菌素6种大环内酯类药物)残留的确证方法。样品用乙腈提取，45℃旋蒸蒸干，再用乙腈-水(1:9，V/V)溶液复溶，PEP-C18混合固相萃取柱净化，氮气吹干后用乙腈定容，超高效液相色谱-串联质谱测定，电喷雾正离子(ESI+)、多反应模式下监测；结果表明，6种药物在5～250μg/kg范围内线性良好(R2＞0.99)，3个添加水平下，6种药物的回收率在60%～99%之间，相对标准偏差为0.2%～8.9%。6种药物的定量限(RSN≥10)均达5.0μg/kg，符合痕量分析的要求。

关键词: 阿维菌素类药物, 固相萃取, 超高效液相色谱-串联质谱

Abstract: A reliable analytical method to determine 6 avermectin residues in 10 foods was developed using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile, evaporated in a rotary evaporator until dryness, re-dissolved in a mixture of acetonitrile and water (1:9, V/V), cleaned up on a PEP-C18 cartridge, blown under nitrogen gas until dryness, and then re-dissolved in acetonitrile prior to UPLC-MS/MS analysis by positive ion electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. The calibration curves of 6 avermectins were linear in the concentration of 5－250μg/kg (R2＞ 0.99). The average recovery rates at three spiked levels were 60%－99% with relative standard deviations (RSDs) of 0.2%－8.9%. The quantification limits for 6 avermectins (RSN≥10) were slightly lower than 5.0 μg/kg. This analytical method could meet the requirements for trace analysis.

Key words: abamectins, solid phase extraction, ultra-high high performance liquid chromatography-tandem mass spectrometry

中图分类号:

TS207

张文娟1，连庚寅2，郭晓喜2，杨小兰1，宋欢2,*. 超高效液相色谱-串联质谱法测定10种食品中的阿维菌素类药物残留[J]. 食品科学, 2012, 33(18): 226-231.

参考文献

参考文献
[1] SHERRATT T N, MACDOUGALL A D, WRATTEN S D, et al. Models to assist the evaluation of the impact of avermectins on dung insect populations[J]. Ecological Modelling, 1998,110(2):165-173.
[2] BERENDSEN B J A, MULDER P P J, VAN RHIJN H J A. The derivatisation of avermectins and milbemycins in milk: New insights and improvement of the procedure[J]. Analytica Chimica Acta, 2007,585(1):126-133.
[3] VIRANT CELESTINA T, KOLAR L, GOBEC I, et al. Factors influencing dissipation of avermectins in sheep faeces[J]. Ecotoxicology and Environmental Safety, 2010,73(1):18-23.
[4] 陈静, 罗永煌. 阿维菌素类药物在动物性食品中的残留检测研究概况[J]. 贵州畜牧兽医, 2007,31(4):9-11.
[5] KOLAR L, FLAJS V C, KUZNER J, et al. Time profile of abamectin and doramectin excretion and degradation in sheep faeces[J]. Environmental PollutionSoil and Sediment Remediation (SSR) - Soil and Sediment Remediation (SSR), 2006,144(1):197-202.
[6] SEELANAN P, SRISA-ART M, PETSOM A, et al. Determination of avermectins in commercial formulations using microemulsion electrokinetic chromatography[J]. Analytica Chimica Acta, 2006,570(1):8-14.
[7] 孙世伟, 李修炼, 李科明, 等. 黄精中阿维菌素残留量检测方法研究[J]. 西北植物学报, 2007,27(6):5.
[8] 赵莉, 谢显传, 占绣萍, 等. 高效液相色谱-荧光法同时检测蔬菜中阿维菌素、甲氨基阿维菌素苯甲酸盐和伊维菌素的多残留量[J]. 中国农业科学, 2010,43(16).
[9] 谢显传, 张少华, 王冬生, 等. 柱前衍生高效液相色谱法测定果蔬产品阿维菌素及其有毒代谢物的残留量[J]. 中国农业科学, 2005,38(11):7.
[10] 赵卫东, 郑文杰, 贺艳, 等. 酶联免疫法检测动物源性产品中阿维菌素残留[J]. 食品研究与开发, 2009,30(4):4.
[11] 杨方, 杨守深, 林永辉, 等. 超高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中阿维菌素类药物残留[J]. 色谱, 2009,27(2):5.
[12] BENINCASA C, PERRI E, IANNOTTA N, et al. LC/ESI-MS/MS method for the identification and quantification of spinosad residues in olive oils[J]. Food Chemistry, 2011,125(3):1116-1120.
[13] 郑卫东, 胡江涛, 阴文娅, 等. 高效液相色谱-串联质谱测定猪肝中阿维菌素、伊维菌素残留[J]. 食品科学, 2011(04):185-188.
[14] 高华鹏, 张健玲, 李永夫, 等. 超高效液相色谱-串联质谱法快速测定鳗鱼中阿维菌素类农药残留[J]. 质谱学报, 2008,29(6):6.
[15] 赵东豪, 贺利民, 聂建荣, 等. 猪肉组织中阿维菌素类药物残留的高效液相色谱-串联质谱法测定[J]. 分析测试学报, 2008,27(8):862-865.