QuEChERS-高效液相色谱-串联质谱法测定多果定在黄瓜和土壤中的残留及消解动态

发布时间：2018-01-16 23:00

本文关键词：QuEChERS-高效液相色谱-串联质谱法测定多果定在黄瓜和土壤中的残留及消解动态　出处：《环境化学》2017年10期 　论文类型：期刊论文

【摘要】：建立了黄瓜和土壤样品中多果定的Qu ECh ERS-高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法,样品经甲醇(乙腈+甲醇)溶液,Qu ECh ERS方法净化,以Agilent ZORBAX Eclipse Plus C_(18)(2.1 mm×50 mm,1.8μm Rapid Resolution HD)色谱柱进行高效液相色谱分离,以电喷雾离子串联质谱正离子(ESI+)多反应监测(MRM)模式进行测定.多果定在黄瓜和土壤上的最低检出浓度(LOQ)为0.01 mg·kg~(-1),平均回收率为77.7%—113.4%,相对标准偏差(RSD)为1.5%—8.0%;多果定在黄瓜和土壤上的残留消解动态规律符合一级动力学方程,其半衰期分别为2.3—4.3 d和2.7—17.3 d.该方法样品前处理简单快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于黄瓜和土壤中多果定残留的检测.
[Abstract]:A high performance liquid chromatography-electrospray tandem mass spectrometry (HPLC-ESI-MS / MS) method was developed for the determination of Doguodine in cucumber and soil samples. The samples were purified by ECh ERS method with methanol (acetonitrile methanol) solution. Agilent ZORBAX Eclipse Plus C _ (18) was taken as 2.1mm 脳 50mm. 1. 8 渭 m Rapid Resolution chromatography column was used for separation by high performance liquid chromatography (HPLC). The method of electrospray ionization tandem mass spectrometry (ESI) multiple reaction monitoring (MRM) model was used. The lowest detectable concentration (LOQ) was determined in cucumber and soil. Was 0.01 mg 路kg ~ (-1). The average recovery was 77.7- 113.4, and the relative standard deviation (RSDs) was 1.5- 8.0; The dynamic law of residue digestion on cucumber and soil accords with the first-order kinetic equation with half-life of 2.3-4.3 days and 2.7-17.3 days respectively. The pretreatment of the sample by this method is simple and rapid. The analytical time, sensitivity, accuracy and precision are all in line with the requirements of pesticide residue detection, which is suitable for the detection of polygoadine residues in cucumber and soil.
【作者单位】：广西大学农药与环境毒理研究所广西农业环境与农产品安全重点实验室培育基地;
【基金】：国家重点研发计划项目(2016YFD0201208-4) 广西农业环境与农产品安全重点实验室培育基地项目(桂科基字[2016]133号)资助~~
【分类号】：O657.63;TS255.7;X833
【正文快照】： 多果定(dodine)又名醋酸十二胍,以氰胺和十二烷基伯胺为原料合成,是一种用途广泛的新型阳离子表面活性剂[1],同时也是一种保护性和非内吸性杀菌剂,其杀菌机制是破坏细胞的渗透性,导致细胞内含物的外渗和细胞死亡[2-4].目前,多果定主要用于防治果树、蔬菜、坚果、观赏植物和成

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