| 高效液相色谱-串联质谱法测定黄瓜与土壤中烯酰吗啉和氰霜唑及其代谢物的残留量 |
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| 基金项目:农业行业标准制定项目（953）；国家重点研发计划项目（SQ2017YFZG20044） |
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| 中文摘要:为评价烯酰吗啉和氰霜唑在黄瓜和土壤中的安全性，建立了同时检测烯酰吗啉和氰霜唑及其代谢物4-氯-5-（4-甲苯基）-1H-咪唑-2-腈（CCIM）的高效液相色谱-串联质谱法。样品经乙腈提取，乙二胺-N-丙基硅烷键合相（PSA）和十八烷基硅烷键合相（C18）净化后，质谱多反应监测模式扫描，基质匹配标准曲线外标法定量。烯酰吗啉、氰霜唑和CCIM在0.01～0.5 mg/L范围内均具有良好的线性关系，相关系数（r）均大于0.994 0，在0.05、0.1、0.5 mg/kg加标浓度下，3种待测物在黄瓜和土壤中的平均回收率为78%~105%，相对标准偏差（RSD）为1.3%～14.8%，定量下限为005 mg/kg。对35%氰霜唑·烯酰吗啉悬浮剂在黄瓜和土壤中的残留动态及最终残留量进行分析，发现烯酰吗啉、氰霜唑及CCIM之和在黄瓜和土壤中消解较快，烯酰吗啉在黄瓜和土壤中的半衰期分别为1.2～2.1、3.0～9.6 d；氰霜唑及CCIM之和在黄瓜和土壤中的半衰期为0.9～2.3、1.8～6.2 d。该方法简单、快速、灵敏度及准确度高，能够满足黄瓜和土壤中烯酰吗啉、氰霜唑及CCIM残留量的检测要求。 |
| 中文关键词:烯酰吗啉 氰霜唑 代谢物 黄瓜 土壤 高效液相色谱-串联质谱法（HPLC-MS/MS） |
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| Determination of Dimethomorph，Cyazofamid and Its Metabolite Residue in Cucumber and Soil Using High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:In order to evaluate the safety of dimethomorph and cyazofamid in cucumber and soil，a high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was developed for the simultaneous detection of dimethomorph，cyazofamid and its metabolite，4-chloro-5-p-tolylimidazole-2-carbonitrile（CCIM） in cucumber and soil.Samples were extracted with acetonitrile，cleaned up with PSA and C18，and then analyzed by HPLC-MS/MS in multiple reaction monitoring（MRM） mode with the matrix matched calibrations method.There existed good linearities for All analytes in the range of 0.01- 0.5 mg/L with their correlation coefficients（r） more than 0.994 0.At three spiked levels of 0.05，0.1 and 0.5 mg/kg，the recoveries for dimethomorph，cyazofamid and CCIM in cucumber and soil were in the range of 78%-105%with relative standard deviations（RSDs） of 1.3%-14.8%.The limit of quantitation was 0.05 mg/kg.Residues and dissipation of dimethomorph and cyazofamid in cucumber and soil were investigated.The half lives of dimethomorph in cucumber and soil were 1.2-2.1 d and 3.0-9.6 d，respectively，and the half lives of cyazofamid and CCIM in cucumber and soil were 0.9-2.3 d and 1.8-6.2 d，respectively.The method is simple，rapid，sensitive and accurate，and could meet the requirements for detection of dimethomorph，cyazofamid and CCIM residues in cucumber and soil. |
| Key Words:dimethomorph cyazofamid metabolite cucumber soil high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） |
| 引用本文：赵民娟,郭虹娜,邵华,金芬,金茂俊,佘永新,王珊珊,郑鹭飞,王静.高效液相色谱-串联质谱法测定黄瓜与土壤中烯酰吗啉和氰霜唑及其代谢物的残留量[J].分析测试学报,2018,37(11):1316-1321. |
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