QuEChERS-高效液相色谱-串联质谱法测定高粱中吡蚜酮残留和消解动态  

Residue and dissipation dynamics of pymetrozine in sorghum by QuEChERS and high performance liquid chromatography-tandem mass spectrometry

作　　者：郑坤明 陈冬花 徐佳 张钰萍 苏建峰 胡德禹[2] ZHENG Kunming;CHEN Donghua;XU Jia;ZHANG Yuping;SU Jianfeng;HU Deyu(Fujian CCIC-Faifrreach Food Safety Testing Co.,Ltd、Fuzhou 350028,China;Research and Development Center for Fine Chemicals,State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering,Key Laboratory of Green Pesticide and Agricultural Bioengineering,Ministry of Education,Guizhou University,Guiyang 550025,China)

机构地区：[1]福建中检华日食品安全检测有限公司,福州350028 [2]贵州大学精细化工研究开发中心,绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室,贵阳550025

出　　处：《农药学学报》2020年第6期1104-1108,共5页Chinese Journal of Pesticide Science

基　　金：国家自然科学基金(21667007)。

摘　　要：建立了高粱Sorghum bicolor(L.)Moench籽粒及高梁植株中吡蚜酮残留的QuEChERS-高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经0.1%甲酸-乙腈提取,通过乙二胺-N-丙基硅烷(PSA)和十八烷基键合硅胶(C18)分散萃取净化,采用电喷雾离子化正离子扫描(ESI+)和多反应监测模式(MRM)检测,外标法定量。结果表明:在0.001~0.2 mg/L范围内,吡蚜酮质量浓度与对应的峰面积间线性关系良好,R2≥0.9970。在0.002、0.02和0.2 mg/kg添加水平下,吡蚜酮在高粱和高粱植株中的日内平均回收率为71%~92%,日内相对标准偏差(RSD)(n=5)为0.8%~5.6%;日间平均回收率为71%~96%,日间RSD(n=15)为1.2%~4.2%。吡蚜酮在高粱籽粒和高粱植株中的定量限(LOQ)均为0.002 mg/kg。消解动态试验结果表明,吡蚜酮在高粱植株中的消解动态符合一级反应动力学方程,在内蒙古和黑龙江2个试验点的高粱植株中的消解半衰期分别为9.7 d和9.0 d。该方法可用于高粱中痕量吡蚜酮残留的检测。这些数据有助于高粱中吡蚜酮最大残留限量的制定,并指导吡蚜酮在高粱上的合理使用。A QuEChERS method with high performance liquid chromatography-tandem mass spectrometry(HPLC–MS/MS)was developed and validated to simultaneously determine pymetrozine in sorghum and its straw.The samples were extracted from sorghum and its straw with acetonitrile containing 0.1%acetic acid,and the extracts were purified by PSA and C18 column.The samples were then detected by the HPLC-MS/MS using positive ions electrospray scanning with multiple reaction monitoring mode.The matrix-matched external standard calibration curves were used for quantitative analysis.The satisfactory linearity(R2≥0.9970)of this method was obtained for sorghum and its straw in the range of 0.001-0.2 mg/L.The intra-day average recoveries of pymetrozine in spiked samples with fortified levels of 0.002,0.02 and 0.2 mg/kg were between 71%and 92%,and the relative standard deviation(RSD)ranged from 0.8%to 5.6%(n=5).The inter-day average recoveries ranged from 71%to 96%and the RSD ranged from 1.2%to 4.2%(n=15).The limits of quantification for pymetrozine in sorghum and its straw were both 0.002 mg/kg.The dissipation dynamics of pymetrozine in sorghum straw followed the first order kinetics equations,and its dissipation half-lives in the Inner Mongolia and Heilongjiang were 9.7 d and 9.0 d,respectively.The results indicated that the established method could be used to detect trace amounts of pymetrozine in sorghum.The data could also help to establish the maximum residue limits of pymetrozine on sorghum and establish the proper and safe usage of pymetrozine on sorghum plants.

关 键 词：QUECHERS 高效液相色谱-串联质谱 高梁 吡蚜酮 残留 消解动态 

分 类 号：S482.3[农业科学—农药学] O657.63[农业科学—植物保护]