QuEChERS-液相色谱-串联质谱法同时检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的残留

引用本文: 李福琴, 石丽红, 王飞, 孙财远, 康頔, 张钰萍, 陈泠竹, 胡德禹. QuEChERS-液相色谱-串联质谱法同时检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的残留[J]. 色谱, 2017, 35(6): 620-626. doi: 10.3724/SP.J.1123.2017.01031 shu

Citation: LI Fuqin, SHI Lihong, WANG Fei, SUN Caiyuan, KANG Di, ZHANG Yuping, CHEN Lingzhu, HU Deyu. Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(6): 620-626. doi: 10.3724/SP.J.1123.2017.01031 shu

QuEChERS-液相色谱-串联质谱法同时检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的残留

贵州大学精细化工研究开发中心, 教育部绿色农药与农业生物工程国家重点实验室, 贵州贵阳 550025
基金项目:
贵州大学研究生创新基金项目（2016077）.

摘要: 建立了QuEChERS-液相色谱-串联质谱法（LC-MS/MS）检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的分析方法。样品经甲醇或乙腈提取，N-丙基乙二胺（PSA）净化后，用液相色谱分离，电喷雾正离子多反应监测（MRM）模式进行质谱测定，以基质匹配标准溶液进行外标法定量。吡唑醚菌酯、甲基硫菌灵和多菌灵的定量限（LOQ，S/N=10）分别为5.8~7.0 μg/kg、9.3~14.1 μg/kg和2.1~2.6 μg/kg。样品的加标回收率为75.48%~109.18%，相对标准偏差（RSD）为0.60%~5.11%（n=5）。该法快速简便，定量准确，用基质配制标准溶液能够有效、准确地校正LC-MS/MS测定吡唑醚菌酯、甲基硫菌灵和多菌灵残留的基质效应，满足土壤、橘皮、橘肉和柑橘全果实际样品的检测需求。

关键词:

English

Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry

Research and Development Center for Fine Chemicals, State Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education, Guizhou University, Guiyang 550025, China
Received Date: 22 January 2017
Fund Project:
Guizhou University Graduate Student Innovation Fund (No. 2016077).

Abstract: A QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of pyraclostrobin, thiophanate-methyl and its metabolite carbendazim in soil and citrus. The samples were extracted with methanol or acetonitrile, purified by primary secondary amine (PSA), then separated by LC, detected in multiple reaction monitoring (MRM) mass spectrometry mode via positive electrospray ionization. The analytes were quantified by matrix-matched standard solutions with external standard method. The limits of quantification (LOQs) of pyraclostrobin, thiophanate-methyl and carbendazim in different matrices were 5.8-7.0 μg/kg, 9.3-14.1 μg/kg and 2.1-2.6 μg/kg, respectively. For all the samples, the spiked recoveries ranged from 75.48% to 109.18%, and the relative standard deviations (RSDs) were 0.60%-5.11% (n=5). The method is quick, easy, effective, sensitive and accurate. The matrix-matched calibration solutions can efficiently compensate matrix effects of the pyraclostrobin, thiophanate-methyl and carbendazim in LC-MS/MS analysis. The established method can be applied to the residue analysis of the real samples of soil, citrus peel, citrus pulp and citrus fruits.

Key words:

liquid chromatography-tandem mass spectrometry (LC-MS/MS)
/ QuEChERS
/ pyraclostrobin
/ thiophanate-methyl
/ carbendazim
/ soil
/ citrus

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沈阳化工大学材料科学与工程学院沈阳 110142

QuEChERS-液相色谱-串联质谱法同时检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的残留

English

Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

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QuEChERS-液相色谱-串联质谱法同时检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的残留

English

Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography- tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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