液相色谱-质谱联用检测农产品中磺草灵残留

doi:10.7506/spkx1002-6630-201322056

食品科学 ›› 2013, Vol. 34 ›› Issue (22): 277-280.doi: 10.7506/spkx1002-6630-201322056

液相色谱-质谱联用检测农产品中磺草灵残留

张启凤，松本和雄，张茂强，姜健美，赵华锋

1.青岛诚誉食品检测有限公司，山东青岛 266108；2.株式会社亚细亚食品安全研究中心，东京 1040045

收稿日期:2013-01-21 修回日期:2013-10-23 出版日期:2013-11-25 发布日期:2013-12-05
通讯作者: 张启凤 E-mail:zhangqf@chengyu.cn

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

ZHANG Qi-feng，KAZUO Matsumoto，ZHANG Mao-qiang，JIANG Jian-mei，ZHAO Hua-feng

1. Qingdao Chengyu Food Testing Laboratory Co. Ltd., Qingdao 266108, China；
2. Asia Food Safety Research Center Inc., Tokyo 1040045, Japan

Received:2013-01-21 Revised:2013-10-23 Online:2013-11-25 Published:2013-12-05
Contact: Qi-Feng ZHANG E-mail:zhangqf@chengyu.cn

摘要/Abstract

摘要：

建立农产品中前处理操作简单，易于进行液相色谱-质谱联用测定的磺草灵残留检测方法。用甲醇提取目标物，分取一定量的溶液进行浓缩，再用含1%乙二胺四乙酸二钠盐(EDTANa2)的0.1%甲酸溶液溶解。将溶解后的样品加载到预先平衡好的亲水亲脂平衡反相固相萃取柱(HLB)上，磺草灵则被保留在HLB上的吸附剂中。经淋洗后用50%甲醇溶液洗脱。将接收溶液用0.45μm的滤膜过滤至进样瓶中，用LC-MS-MS进行测定。6种农产品基体的平均回收率为70.6%～107.8%，相对标准偏差为1.0%～14.0%，日间精密度为4.4%～17.7%，基质回收率为81.4%～115.0%，基质效应影响不大。经实验验证，方法定量限为0.01mg/kg，精密度、灵敏度满足检测要求，操作简便、快捷，可用于农产品中磺草灵的残留检测。

关键词: 磺草灵, 残留检测, 固相萃取柱, 液相色谱-质谱联用, 农产品

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

中图分类号:

TS207.3

张启凤，松本和雄，张茂强，姜健美，赵华锋. 液相色谱-质谱联用检测农产品中磺草灵残留[J]. 食品科学, 2013, 34(22): 277-280.

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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液相色谱-质谱联用检测农产品中磺草灵残留

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

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