Determination of Asulam in Agricultural Products by LC-MS-MS

doi:10.7506/spkx1002-6630-201322056

Abstract

Abstract:

A simplified pretreatment coupled with reliable liquid chromatography-tandem mass spectrometry (LC-MS-MS)
method has been developed for the determination of asulam in agricultural products. Samples were extracted with methanol,
and then divided into equal portions. After evaporation, residues were dissolved in 0.1% formic acid solution containing 1%
disodium ethylenediamine tetraacetic acid (EDTANa2). The sample was applied to a pre-conditioned hydrophilic lipophilic
balanced reversed solid-phase extraction column (HLB). Under these conditions, asulam was retained in the adsorbent of
HLB. After flushing of the column, asulam was eluted with 50% methanol solution. It was filtered through a 0.45 μm filter
to a vial before analysis by LC-MS-MS. The average recoveries from 6 agricultural samples varied from 70.6% to 107.8%,
the repeatability varied from 1.0% to 14.0%, the inter-day precision varied from 4.4% to 17.7% and the matrix recoveries
varied from 81.4% to 115.0%, showing little matrix effect. The validation experiments showed that the method was simple,
fast, accurate and sensitive and could meet the requirements for the determination and confirmation of asulam in agricultural
products with a limit of quantification of 0.01 mg/kg.

Key words: asulam, determination, solid-phase extraction column, liquid chromatography-tandem mass spectrometry (LC-MS-MS), agricultural products

CLC Number:

TS207.3

ZHANG Qi-feng，KAZUO Matsumoto，ZHANG Mao-qiang，JIANG Jian-mei，ZHAO Hua-feng. Determination of Asulam in Agricultural Products by LC-MS-MS[J]. FOOD SCIENCE, 2013, 34(22): 277-280.

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