Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, China.
Anal Bioanal Chem. 2011 Mar;399(7):2539-47. doi: 10.1007/s00216-010-4606-7. Epub 2011 Jan 8.
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.
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。