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超高效液相色谱-串联质谱法快速分析土壤、水和小麦中四种三唑并嘧啶类除草剂残留

Rapid residue analysis of four triazolopyrimidine herbicides in soil, water, and wheat by ultra-performance liquid chromatography coupled to tandem mass spectrometry.

机构信息

Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, China.

出版信息

Anal Bioanal Chem. 2011 Mar;399(7):2539-47. doi: 10.1007/s00216-010-4606-7. Epub 2011 Jan 8.

Abstract

A sensitive and effective method for simultaneous determination of triazolopyrimidine sulfonamide herbicide residues in soil, water, and wheat was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry. The four herbicides (pyroxsulam, flumetsulam, metosulam, and diclosulam) were cleaned up with an off-line C18 SPE cartridge and detected by tandem mass spectrometry using an electrospray ionization source in positive mode (ESI+). The determination of the target compounds was achieved in <2.0 min. The limits of detection were below 1 μg kg(-1), while the limits of quantification did not exceed 3 μg kg(-1) in different matrices. Quantitation was determined from calibration curves of standards containing 0.05-100 μg L(-1) with r(2) > 0.997. Recovery studies were conducted at three spiked levels (0.2, 1, and 5 μg kg(-1) for water; 5, 10, and 100 μg kg(-1) for soil and wheat). The overall average recoveries for this method in water, soil, wheat plants, and seeds at three levels ranged from 75.4% to 106.0%, with relative standard deviations in the range of 2.1-12.5% (n = 5) for all analytes.

摘要

建立了一种超高效液相色谱-串联质谱法,用于同时测定土壤、水和小麦中三唑并嘧啶磺酰胺类除草剂残留。采用离线 C18 SPE 小柱净化,电喷雾源正离子模式(ESI+)串联质谱检测,4 种除草剂(吡氟酰草胺、氟唑磺隆、唑嘧磺草胺、啶磺草胺)可在<2.0 min 内完成测定。不同基质中,目标化合物的检出限均低于 1μg kg(-1),定量限均不超过 3μg kg(-1)。在 0.05-100μg L(-1)浓度范围内,标准曲线的相关系数(r(2))均大于 0.997。在水、土壤和小麦中分别以 0.2、1 和 5μg kg(-1),5、10 和 100μg kg(-1) 3 个添加水平进行了回收率研究。该方法在水、土壤、小麦植株和种子中的平均回收率为 75.4%-106.0%,相对标准偏差(RSD)在 2.1%-12.5%(n = 5)范围内。

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