色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1276-1285.DOI: 10.3724/SP.J.1123.2017.09019

• 研究论文 • 上一篇    下一篇

改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中7种阿维菌素类药物残留

刘永涛1,2, 余琳雪1,3, 王桢月1,3, 杨秋红1,2, 董靖1,2, 杨移斌1,2, 艾晓辉1,2   

  1. 1. 中国水产科学研究院长江水产研究所, 湖北 武汉 430223;
    2. 农业部水产品质量安全控制重点实验室, 北京 100141;
    3. 上海海洋大学水产与生命学院, 上海 201306
  • 收稿日期:2017-09-09 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 艾晓辉,Tel:(027)81780298,E-mail:thincat2005@sina.com
  • 基金资助:

    公益性行业（农业）科研专项（201503108）；农业行业标准制修订项目（2015-152，2014-443）；中央级公益性科研院所基本科研业务费专项资金（2016JBF0104）.

Simultaneous determination of seven avermectin residues in aquatic products by modified QuEChERS combined with high-performance liquid chromatography-tandem mass spectrometry

LIU Yongtao1,2, YU Linxue1,3, WANG Zhenyue1,3, YANG Qiuhong1,2, DONG Jing1,2, YANG Yibin1,2, AI Xiaohui1,2   

  1. 1. Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan 430223, China;
    2. Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing 100141, China;
    3. College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, China
  • Received:2017-09-09 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Special Fund for Agro-Scientific Research in the Public Interest (No. 201503108); Agricultural Industry Standard System Formulation and Revision Project (Nos. 2015-152, 2014-443); Central Public-Interest Scientific Institution Basal Research Fund (No. 2016JBF0104).

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312

被引次数

2

摘要：

建立了改良的QuEChERS结合高效液相色谱-串联质谱（HPLC-MS/MS）同时测定水产品中7种阿维菌素类药物（阿维菌素、伊维菌素、多拉菌素、塞拉菌素、乙酰氨基阿维菌素、莫西菌素和埃玛菌素）的分析方法。样品经0.2%（v/v）氨化乙腈提取，3 g无水硫酸镁和2 g无水硫酸钠除水剂和沉淀蛋白质，100 mg十八烷基硅烷（C18）和500 mg无水硫酸镁净化。以0.1%（v/v）甲酸乙腈（含5 mmol/L乙酸铵）-0.1%（v/v）甲酸水溶液（含5 mmol/L乙酸铵）为流动相，采用Varian Pursuit ULTRA C8色谱柱（100 mm×2.0 mm，2.8 μm）进行分离。在加热电喷雾离子（HESI）源、正离子模式下采用多反应监测模式检测，基质匹配标准曲线外标法定量。阿维菌素、伊维菌素、多拉菌素、塞拉菌素、乙酰氨基阿维菌素和莫西菌素在2~200 μg/L范围内、埃玛菌素在0.2~20 μg/L范围内呈线性相关，相关系数（r）均≥ 0.9972，水产品中阿维菌素类药物的加标回收率为71.6%~112.8%，相对标准偏差（RSD）为4.7%~13.1%，不同水产品的基质效应均小于15%。阿维菌素、伊维菌素、多拉菌素、塞拉菌素、乙酰氨基阿维菌素和莫西菌素的定量限均为5 μg/kg，埃玛菌素的定量限为0.25 μg/kg。该法操作简便，重复性好，适用于水产品中7种阿维菌素类药物残留量的同时测定。

关键词: QuEChERS, 阿维菌素类药物, 残留, 高效液相色谱-串联质谱, 水产品

Abstract:

A method was established for the simultaneous determination of seven avermectin (AVMs) residues, such as avermectin, ivermectin, doramectin, selamectin, eprinomectin, moxidectin and emamectin, in aquatic products using modified QuEChERS and high-performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with 0.2% (v/v) ammoniate acetonitrile, and then 3 g of anhydrous magnesium sulfate and 2 g of anhydrous sodium sulfate were added to remove moisture and precipitate proteins. The samples were purified with 100 mg of C18 and 500 mg of anhydrous magnesium sulfate. The mobile phases comprised of acetonitrile (containing 0.1% (v/v) formic acid and 5 mmol/L ammonium acetate) and water (containing 0.1% (v/v) formic acid and 5 mmol/L ammonium acetate). The prepared samples were separated on a Varian Pursuit ULTRA C8 column (100 mm×2.0 mm, 2.8 μm) and determined using heated electrospray ionization (HESI) in the positive ion multiple reaction monitoring (MRM) mode. The analytes were quantified using external standard with the matrix-matched standard calibration curve method. The results showed that the solvent and matrix-matched standard curves for avermectin, ivermectin, doramectin, selamectin, eprinomectin and moxidectin in the range of 2-200 μg/L and for emamectin in the range of 0.2-20 μg/L were all linear, and the correlation coefficients (r) were ≥ 0.9972. The recoveries were 71.6%-112.8% with the relative standard deviations in the range of 4.7%-13.1%. The limits of quantification (LOQs) for avermectin, ivermectin, doramectin, selamectin, eprinomectin and moxidectin were all 5 μg/kg and for emamectin was 0.25 μg/kg. The present method is simple, repeatable, and suitable for the simultaneous determination of the residues of the seven avermectins in aquatic products.

Key words: aquatic products, avermectins (AVMs), high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), QuEChERS, residue

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