QuEChERS-超高效液相色谱-串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂

doi:10.3724/SP.J.1123.2018.02020

色谱 ›› 2018, Vol. 36 ›› Issue (8): 730-737.DOI: 10.3724/SP.J.1123.2018.02020

QuEChERS-超高效液相色谱-串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂

王璐芳^1,2, 李春梅², 许佳彬¹, 李慧¹, 苏杭², 王静², 金芬², 张宇¹

1. 海南大学热带农林学院, 海南海口 570228;
2. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081

收稿日期:2018-02-11 出版日期:2018-08-08 发布日期:2014-06-28
通讯作者: 金芬,E-mail:jinfen2017@gmail.com;张宇,E-mail:yuzhang_rain@163.com
基金资助:
基本科研业务费专项重大平台推进计划（Y2017PT37）；基本科研业务费人才引导项目（1610072016004）；中国农业科学院"科研英才培育工程"项目.

Simultaneous determination of 11 strobilurin fungicides in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

WANG Lu-fang^1,2, LI Chun-mei², XU Jiabin¹, LI Hui¹, SU Hang², WANG Jing², JIN Fen², ZHANG Yu¹

1. Institute of Tropical Agriculture and Forestry, Hainan University, Haikou 570228, China;
2. Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China

Received:2018-02-11 Online:2018-08-08 Published:2014-06-28
Supported by:
Special Funds of Basic Scientific Research Expenses for Major Platform Promotion Project (No.Y2017PT37);Special Funds of Basic Scientific Research Expenses for Talent Guide Project (No.1610072016004);"Scientific Research Talents Cultivation Project" of Chinese Academy of Agricultural Sciences.

摘要/Abstract

摘要：

建立了同时检测6种不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂（丁香菌酯、氯啶菌酯、啶氧菌酯、氟嘧菌酯、肟菌酯、E-苯氧菌胺、醚菌酯、醚菌胺、肟醚菌胺、唑菌酯和烯肟菌胺）的QuEChERS-超高效液相色谱-串联质谱分析方法。土壤样品经0.1%（体积分数）醋酸乙腈提取，用100 mg N-丙基乙二胺（PSA）和100 mg C₁₈净化。采用C₁₈色谱柱进行色谱分离和分析，以甲醇和水为流动相进行梯度洗脱，以电喷雾正离子、多反应监测模式进行定性分析，采用基质标准曲线外标法进行定量分析。结果表明：11种甲氧基丙烯酸酯杀菌剂在0.1~100 μg/kg范围内线性关系良好，相关系数为0.9805~0.9999。空白样品在5、10和50 μg/kg添加水平下的平均回收率为65.1%~103.9%，相对标准偏差为0.082%~14%（n=3），定量限为0.005~2.0 μg/kg。该方法能够满足不同植被类型土壤（黑土、红壤土、砂土、潮土、灰漠土、高山土）中11种甲氧基丙烯酸酯类杀菌剂痕量检测的要求。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 甲氧基丙烯酸酯类杀菌剂, 土壤

Abstract:

A method for the simultaneous determination of the 11 strobilurin fungicides (coumoxystrobin, tricyclopyricarb, picoxystrobin, fluoxastrobin, trifloxystrobin, E-metominostrobin, kresoxim-methyl, dimoxystrobin, orysastrobin, pyraoxystrobin and fenaminstrobin) in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry was developed. The strobilurin fungicides were extracted with 0.1% (volume percentage) acetic acid-acetonitrile, and cleaned-up with 100 mg primary secondary amine (PSA) and 100 mg C₁₈. The separation was performed on a C₁₈ column with methanol and water as the mobile phases. The strobilurin fungicides were determined in the positive ion mode and multiple reaction monitoring mode. The quantification was carried out by the matrix-matched external standard curve. The results showed good linear relationships for all analytes in the range of 0.1-100 μg/kg with the correlation coefficients of 0.9805-0.9999. The mean recoveries of strobilurin fungicides in the spiked soil samples were 65.1%-103.9% and the relative standard deviations were 0.082%-14% (n=3) at three spiked levels (5, 10 and 50 μg/kg). The limits of quantitation were 0.005-2.0 μg/kg. This method is suitable for the trace determination of the 11 strobilurin fungicides in different vegetation types of soil (black soil, red soil, sandy soil, moisture soil, desert grey soil, and plateau soil).

Key words: QuEChERS, soil, strobilurin fungicides, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

王璐芳, 李春梅, 许佳彬, 李慧, 苏杭, 王静, 金芬, 张宇. QuEChERS-超高效液相色谱-串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂[J]. 色谱, 2018, 36(8): 730-737.

WANG Lu-fang, LI Chun-mei, XU Jiabin, LI Hui, SU Hang, WANG Jing, JIN Fen, ZHANG Yu. Simultaneous determination of 11 strobilurin fungicides in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(8): 730-737.

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QuEChERS-超高效液相色谱-串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂

Simultaneous determination of 11 strobilurin fungicides in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

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