高效液相色谱串联质谱法测定葡萄中精甲霜灵、吡唑醚菌酯、氰霜唑及其代谢物CCIM残留  

Determination of Metalaxyl-M,Pyraclostrobin, Cyazofamid and CCIM in Grape by HPLC-MS/MS

作　　者：黄鑫 贾福艳[1,2] 刘良月 关鑫[1,2] 杨沛文 郭红霞 张双 杨雪葳 黄成田 Huang Xin;Jia Fuyan;Liu Liangyue;Guan Xin;Yang Peiwen;Guo Hongxia;Zhang Shuang;Yang Xuewei;Huang Chengtian(Shenyang SYRICI Testing Co.,Ltd.,Shenyang Liaoning 110021,China;Shenyang Research Institute of Chemical Industry Co.,Ltd.,Shenyang Liaoning 110021,China)

机构地区：[1]沈阳沈化院测试技术有限公司,辽宁沈阳110021 [2]沈阳化工研究院有限公司,辽宁沈阳110021

出　　处：《农药科学与管理》2022年第2期31-36,共6页Pesticide Science and Administration

摘　　要：建立高效液相色谱串联质谱测定葡萄中精甲霜灵、吡唑醚菌酯、氰霜唑及其代谢物CCIM的残留分析方法。葡萄中精甲霜灵、吡唑醚菌酯、氰霜唑及CCIM经乙腈(含1%乙酸)振荡提取,氯化钠盐析分离水相和乙腈相,PSA和C_(18)吸附剂净化,HPLC-MS/MS测定。精甲霜灵、吡唑醚菌酯、氰霜唑及其代谢物CCIM在0.001~0.1mg/L范围内均具有较好的线性关系。葡萄中甲霜灵、吡唑醚菌酯、氰霜唑及其代谢物CCIM的平均回收率为83%~92%,相对标准偏差为1.3%~6.7%。方法的最小检出质量分数均为0.01mg/kg。该方法选择性好,灵敏度高,适用于葡萄中精甲霜灵、吡唑醚菌酯、氰霜唑及其代谢物CCIM的残留检测。A HPLC-MS/MS method for the quantitative determination of Metalaxyl-M,Pyraclostrobin,Cyazofamid and CCIM in grape was established.Metalaxyl-M,Pyraclostrobin,Cyazofamid and CCIM were extracted from grape by shaking extraction using acetonitrile(containing 1% acetic acid).Then sodium chlorid was added to separate water and acetonitrile.The acetonitrile phase was purified by PSA and C_(18) absorbents,and determined by HPLC-MS/MS.The results showed that the responses of Metalaxyl-M,Pyraclostrobin,Cyazofamid and CCIM were linear in the range 0.001~0.1 mg/L.The average recoveries of Metalaxyl-M,Pyraclostrobin,Cyazofamid and CCIM in grape were 83%~92%,and the relative standard deviations were 1.3%~6.7%.The limits of quantification were 0.01 mg/kg.The method has good separation and high sensitivity,which is suitable for residue analysis of Metalaxyl-M,Pyraclostrobin,Cyazofamid and CCIM in grape.

关 键 词：葡萄 精甲霜灵 吡唑醚菌酯 氰霜唑 CCIM 高效液相色谱串联质谱 

分 类 号：S482.2[农业科学—农药学] S481.8[农业科学—植物保护]