色谱

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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

杨方1*,杨守深2,林永辉1,郑丹萍2,卢声宇1,黄志强3,张莹3   

  1. 1.Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China; 2.Fujian Agriculture and Forestry University, Fuzhou 350003, China; 3.Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410007, China
  • 收稿日期:2008-09-03 修回日期:2008-11-11 出版日期:2009-03-30 发布日期:1982-12-25
  • 通讯作者: 杨方
  • 基金资助:
    国家“十一五”科技支撑计划项目(No. 2006BAK02A08)

Determination of avermectin residues in tea by ultra-performance liquid chromatography-electrospray tandem mass spectrometry

YANG Fang1*, YANG Shoushen2, LIN Yonghui1, ZHENG Danping2, LU Shengyu1, HUANG Zhiqiang3, ZHANG Ying3   

  1. 1.Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China; 2.Fujian Agriculture and Forestry University, Fuzhou 350003, China; 3.Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410007, China
  • Received:2008-09-03 Revised:2008-11-11 Online:2009-03-30 Published:1982-12-25
  • Contact: YANG Fang1

摘要: 建立了采用超高效液相色谱-电喷雾电离串联质谱同时检测茶叶中爱比菌素、甲胺基阿维菌素、乙酰胺基阿维菌素、伊维菌素、多拉菌素、莫西丁克残留的方法。试样经饱和氯化钠溶液浸润后,用乙腈提取,C18固相萃取小柱净化,超高效液相色谱-电喷雾串联质谱法(UPLC/ESI-MS/MS)测定。对流动相、监测离子、校正曲线等进行了优化和探讨。6种分析物在2.0~50 μg/L范围内线性关系良好,相关系数均大于0.9920。莫西丁克在5,10,20 μg/kg,其余分析物在2,5,10 μg/kg加标水平的平均回收率为61.7%~85.4%,相对标准偏差为9.37%~17.19%。该方法可靠、稳定,可满足茶叶中阿维菌素类药物残留检测与确证的需要。

关键词: 阿维菌素类药物残留, 茶叶 , 超高效液相色谱-质谱联用法

Abstract: A simple and rapid analytical method for the simultaneous determination of abamectin, emamectin, eprinomectin, ivermectin, doramectin and moxidectin residues in tea by ultra-performance liquid chromatography-electrospray tandem mass spectrometry (UPLC/ESI-MS/MS) has been developed. The avermectins were extracted from the tea with acetonitrile after the tea was infiltrated in saturated aqueous NaCl solution, then cleaned up with a C18 solid phase extraction cartridge. The linear ranges were 2.0-50 μg/L and the correlation coefficients were all above 0.9920. Several UPLC-MS/MS conditions that included the mobile phase, monitor ions and the selection of calibration of the measurement were studied . The average recoveries and the relative standard deviations ranged from 61.7% to 85.4% and from 9.37% to 17.19%, respectively, in spiked samples at the concentrations of 5, 10, 20 μg/kg for moxidectin and 2, 5, 10 μg/kg for other analytes. This method is suitable for the determination of avermectin residues in tea.

Key words: avermectin residues, tea , ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)