Liu Yongtao, Yu Linxue, Wang Zhenyue, Yang Qiuhong, Dong Jing, Yang Yibin, Ai Xiaohui
Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan 430223, China.
Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing 100141, China.
Se Pu. 2017 Dec 8;35(12):1276-1285. doi: 10.3724/SP.J.1123.2017.09019.
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 C 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 C 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 () 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.
建立了一种使用改进的QuEChERS和高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定水产品中七种阿维菌素(AVMs)残留量的方法,这七种阿维菌素包括阿维菌素、伊维菌素、多拉菌素、塞拉菌素、依普菌素、莫西菌素和甲氨基阿维菌素苯甲酸盐。样品用0.2%(v/v)氨化乙腈提取,然后加入3 g无水硫酸镁和2 g无水硫酸钠以去除水分并沉淀蛋白质。样品用100 mg C和500 mg无水硫酸镁进行净化。流动相由乙腈(含有0.1%(v/v)甲酸和5 mmol/L乙酸铵)和水(含有0.1%(v/v)甲酸和5 mmol/L乙酸铵)组成。制备好的样品在Varian Pursuit ULTRA C柱(100 mm×2.0 mm,2.8 μm)上进行分离,并采用加热电喷雾电离(HESI)在正离子多反应监测(MRM)模式下进行测定。使用外标法和基质匹配标准曲线法对分析物进行定量。结果表明,阿维菌素、伊维菌素、多拉菌素、塞拉菌素、依普菌素和莫西菌素在2 - 200 μg/L范围内以及甲氨基阿维菌素苯甲酸盐在0.2 - 20 μg/L范围内的溶剂和基质匹配标准曲线均呈线性,相关系数()≥0.9972。回收率为71.6% - 112.8%,相对标准偏差在4.7% - 13.1%范围内。阿维菌素、伊维菌素、多拉菌素、塞拉菌素、依普菌素和莫西菌素的定量限(LOQs)均为5 μg/kg,甲氨基阿维菌素苯甲酸盐的定量限为0.25 μg/kg。本方法简便、可重复,适用于同时测定水产品中七种阿维菌素的残留量。