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采用 HPLC-MS/MS 法,建立了黄瓜和土壤中吡唑醚菌酯及其两种代谢物的快速、简便、廉价、有效、耐用和安全的同时测定方法。

Simultaneous determination of pyrametostrobin and its two metabolites in cucumber and soil using a quick, easy, cheap, effective, rugged, and safe method with HPLC-MS/MS.

机构信息

College of Plant Protection, Shenyang Agricultural University, Shenyang, P. R. China.

Shenyang Research Institute of Chemical Industry, Shenyang, P. R. China.

出版信息

J Sep Sci. 2017 Jun;40(11):2335-2343. doi: 10.1002/jssc.201700109. Epub 2017 May 2.

DOI:10.1002/jssc.201700109
PMID:28387044
Abstract

An easy, effective and sensitive analytical method for the simultaneous determination of a novel fungicide pyrametostrobin and its two metabolites pyrametostrobin-M1 and pyrametostrobin-M2 in cucumber and soil was developed using a quick, easy, cheap, effective, rugged, and safe method with high-performance liquid chromatography and tandem mass spectrometry. The extraction solvent was acetonitrile, and cleanup sorbents were primary secondary amine and graphitized carbon black for cucumber samples and primary secondary amine for soil samples. The three target compounds were successfully separated between 3.2 and 3.9 min using a Waters CORTECS™ C column connected to an electrospray ionization source. All the matrix-matched samples at three fortified levels (10, 100 and 1000  μg/kg) provided satisfactory recoveries in the range of 78.8-93.8% with relative standard deviations below 6.9%. The limits of quantitation for the three compounds were below 0.183 μg/kg. The proposed method was validated by analyzing real samples.

摘要

建立了一种采用高效液相色谱-串联质谱法,以快速、简便、廉价、有效、稳定和安全为特点的分析方法,用于同时测定黄瓜和土壤中新型杀菌剂咯菌腈及其两种代谢物咯菌腈-M1 和咯菌腈-M2。提取溶剂为乙腈,黄瓜样品的净化吸附剂为伯仲胺和石墨化炭黑,土壤样品的净化吸附剂为伯仲胺。采用 Waters CORTECS™ C 柱,连接电喷雾电离源,在 3.2 至 3.9 分钟之间成功分离了 3 种目标化合物。在 3 个加标水平(10、100 和 1000μg/kg)下,所有基质匹配样品的回收率在 78.8-93.8%范围内,相对标准偏差均低于 6.9%。3 种化合物的定量限均低于 0.183μg/kg。通过对实际样品进行分析,验证了该方法的可行性。

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