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,2.8μm)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2~200μg/L范围内、埃玛菌素在0.2~20μg/L范围内呈线性相关,相关系数(r)均≥0.997 2,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5μg/kg,埃玛菌素的定量限为0.25μg/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。
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-performanceliquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted with0.2%(v/v)ammoniate acetonitrile,and then3g of anhydrous magnesium sulfate and2g of anhydrous sodium sulfate were added to remove moisture and precipitate proteins.The samples were purified with100mg of Cl8and500mg of anhydrous magnesium sulfate.Themobile phases comprised of acetonitrile(containing0.1%(v/v)formic acid and5mmol/L ammonium acetate)and water(containing0.1%(v/v)formic acid and5mmol/L ammoniumacetate).The prepared samples were separated on a Varian Pursuit ULTRA C8column(100mmx2.0mm,2.8^m)and determined using heated electrospray ionization(HESI)in the positiveion multiple reaction monitoring(MRM)mode.The analytes were quantified using externalstandard 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 of2-200pg/L and for emamectin in the range of0.2-20pg/L were all linear,and the correlation coefficients(r)were≥0.9972.Therecoveries were71.6%-112.8%with the relative standard deviations in the range of4.7%-13.1%.The limits of quantification(LOQs)for avermectin,ivermectin,doramectin,selamectin,eprinomectin and moxidectin were all5pg/kg and for emamectin was0.25pg/kg.Thepresent method is simple,repeatable,and suitable for the simultaneous determination of theresidues of the seven avermectins in aquatic products.
作者
刘永涛
余琳雪
王桢月
杨秋红
董靖
杨移斌
艾晓辉
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;College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China)
出处
《色谱》
CAS
CSCD
北大核心
2017年第12期1276-1285,共10页
Chinese Journal of Chromatography
基金
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)~~
关键词
高效液相色谱-串联质谱
QUECHERS
残留
阿维菌素类药物
水产品
high-performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS)
QuEChERS
residue
avermectins (AVMs)
aquatic products
