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一种结合超高效液相色谱-串联质谱法,用于同时检测谷物中四种三唑酮类除草剂的快速、简便、廉价、有效、耐用且安全的方法。

A quick, easy, cheap, effective, rugged, and safe method for the simultaneous detection of four triazolone herbicides in cereals combined with ultrahigh performance liquid chromatography with tandem mass spectrometry.

作者信息

Tao Yan, Xu Jun, Liu Xingang, Cheng Youpu, Liu Na, Chen Zenglong, Dong Fengshou, Zheng Yonguan

机构信息

State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, P.R. China.

出版信息

J Sep Sci. 2014 Sep;37(17):2340-8. doi: 10.1002/jssc.201400186. Epub 2014 Jul 15.

Abstract

This paper describes a novel, rapid, and sensitive analytical method for monitoring four triazolone herbicides in cereals (wheat, rice, corn, and soybean), using a quick, easy, cheap, effective, rugged, and safe sample extraction procedure followed by ultrahigh performance liquid chromatography coupled with tandem mass spectrometry. The four triazolone herbicides (amicarbazone, carfentrazone-ethyl, sulfentrazone, and thiencarbazone-methyl) were extracted using acidified acetonitrile (containing 1% v/v formic acid) and subsequently purified with octadecylsilane (C18 ) prior to sample analysis. Ultrahigh performance liquid chromatography coupled with tandem mass spectrometry was operated in positive and negative ionization switching mode. Amicarbazone and carfentrazone-ethyl were detected in the positive mode (ESI+), while sulfentrazone and thiencarbazone-methyl were detected in the negative mode (ESI-). All compounds were successfully separated in less than 3.0 min. Further optimization achieved desired recoveries ranging from 74.5 to 102.1% for all analytes with relative standard deviation values ≤17.2% in all tested matrices at three levels (10, 100, and 500 μg/kg). The limits of detection for all compounds were ≤2.3 μg/kg, and the limits of quantitation did not exceed 7.1 μg/kg. The developed method showed excellent linearity (R(2) ≥ 0.994) and was proven to be highly efficient and reliable for the routine monitoring of triazolone herbicides in cereals.

摘要

本文描述了一种新颖、快速且灵敏的分析方法,用于监测谷物(小麦、水稻、玉米和大豆)中的四种三唑啉酮类除草剂。该方法采用快速、简便、廉价、高效、耐用且安全的样品提取程序,随后结合超高效液相色谱-串联质谱法。四种三唑啉酮类除草剂(氨唑草酮、唑酮草酯、乙氧磺隆和甲基硫菌灵)使用酸化乙腈(含1% v/v甲酸)进行提取,随后在样品分析前用十八烷基硅烷(C18)进行净化。超高效液相色谱-串联质谱法在正、负离子切换模式下运行。氨唑草酮和唑酮草酯在正模式(ESI+)下检测,而乙氧磺隆和甲基硫菌灵在负模式(ESI-)下检测。所有化合物在不到3.0分钟内成功分离。进一步优化后,所有分析物在三个浓度水平(10、100和500 μg/kg)的所有测试基质中的回收率达到74.5%至102.1%,相对标准偏差值≤17.2%。所有化合物的检测限≤2.3 μg/kg,定量限不超过7.1 μg/kg。所建立的方法具有出色的线性(R(2)≥0.994),并被证明对于谷物中三唑啉酮类除草剂的常规监测具有高效性和可靠性。

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