UPLC-MSMS测定葡萄酒中3种双酰胺类杀虫剂.pdfVIP

2016 Vol.35 NO.9 .172. Serial NO.295 China Brewing Analysis and Examination UPLC-MSIMS测定葡萄酒中3种双酷肢类杀虫剂 张云1 ，程立军1 ，侯杰l ，陈泽宇l ，朱海燕2 (1.三明出入境检验检疫局，福建三明 365000; 2. 三明学院资源与化工学院，福建三明 365000) 摘 要:建立了葡萄酒中氟虫酷胶、氯虫苯甲酷胶、氟苯虫酸胶等3种双瞰胶类杀虫剂残留量的超高效液相色谱·串联质谱(upLC­ 固相萃取柱净化，以乙腊 MSIMS)检测方法。葡萄酒中的3种双酸肢类杀虫剂经乙腊提取后，用GCB.刷H -5 mmoJIL乙酸镀·甲酸作为流 2 动相，梯度洗脱，通过UPLC-MSIMS进行测定。结果表明，3种双酸肢类杀虫剂在质量浓度1-20 件WL范围内呈良好的线性关系，相关 系数(R);;:0.9995 ，方法检出限1.0 IJ.glkg; 以1.0μglkg、 2.0 IJ.glkg , 10μglkg为添加水平，平均回收率在76.3%-91.1%之间，相对标准 偏差但SD)为3.9%-9.8%。表明该方法快速简便、净化效果好、准确度较好、精密度较高，可应用于葡萄酒中3种双曹先胶类杀虫剂的同 时测定。 关键词z 葡萄酒:双酸胶类杀虫剂:超高效液相色谱·串联质谱:测定 doi:10.1188剖.i臼n.0254-5071.2016.09.039 申图分类号:0657.7 文章编号:0254-5071(2016)09-0172-04 Determination of也ree kin也ofdiamides insecticides in wine by UPLC-MSIMS ZHANG Yun , CHENG Lij时， HOU Jie , CHEN Zeyul ,zl丑JHaiyan2 ρ. SanmingEn町I-Exit Inspection and Quarantine Bureau, Sanming 365000， αina; 2.Schωi] ofResources and αemicaJEngineering, Sanm吨Univers，取Sanming 3651侃)()， China) Abstract: The detection me也od of three kinds of diamides insecticides (including c归由aniliprole， chloran回niliprole， t1ubendiamide in wine) residu- al amount in wine was established by ultra performance liquid chromaωgraphy tandem m础咿酬。metry (UPLC-MSIMS). The 也ree kinds of di- amides insecticides in wine was extracted by aceωni位ile，姐d 也e extracting solution was pur诅ed by GCB.1NH2ωlid-phωe ex回.ction colurnn, with aceωnitrile-5 mmoJIL ammonium acetate-methanoic acid as mobile phase ,then determined by UPLC-MSIMS after gr叫ient elute. The results show