应用化学 ›› 2010, Vol. 27 ›› Issue (04): 488-493.DOI: 10.3724/SP.J.1095.2010.90362

• 研究论文 • 上一篇    下一篇

蔬菜和食用菌中氨基甲酸酯类农药残留检测技术

姚家彪*,赵颖,潘伟,蒋施,钟钰,金雁   

  1. (沈阳出入境检验检疫局综合技术中心 沈阳 110016)
  • 收稿日期:2009-05-25 修回日期:2009-09-16 出版日期:2010-04-10 发布日期:2010-04-10
  • 通讯作者: 姚家彪,男,研究员; E-mail:yaojiab@lnciq.gov.cn; 研究方向:食品及农副产品中农兽药残留分析及有毒、有害物质分析
  • 基金资助:
    “十一·五”国家科技支撑计划(2006BAK02A08-005)资助项目

Determination of Carbamate Pesticide Residue in Vegetables and Mushrooms

YAO Jia-Biao*, ZHAO Ying, PAN Wei, JIANG Shi, ZHONG Yu, JIN Yan   

  1. (Technology Center,Shenyang EntryExist Inspection and Quarantine Bureau,Shenyang 110016)
  • Received:2009-05-25 Revised:2009-09-16 Published:2010-04-10 Online:2010-04-10

摘要:

建立了丙酮和乙腈(体积比85:15)提取,凝胶渗透色谱(GPC)法和PSA(N-丙基乙二胺)固相萃取柱2种方法净化,超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测菠菜、黄瓜、大葱、蘑菇、香菇、木耳、牛肝菌和胡萝卜中19种氨基甲酸酯类农药,同位素稀释法定量。实验结果表明,GPC法净化,回收率为70.1%~95.7%;PSA固相萃取柱净化,回收率为70.2%~94.9%。方法的检出限均为1×10-5 g/kg。各种NMCs在确定的添加范围内线性关系良好,线性相关系数r均>0.99,所建立的检测方法实用、准确、灵敏度高。

关键词: 超高效液相色谱-串联质谱, 蔬菜, 食用菌, 氨基甲酸酯

Abstract:

A method was developed for the simultaneous determination of 19 carbamate pesticides residues in spinach, cucumber, scallion, fungus, mushroom, agaric and carrot by liquid chromatography tandem mass spectrometry(UPLCMS/MS) combined with isotope internal standard method. The vegetable and mushroom samples were extracted with V(acetone)∶V(acetonitrile)=85∶15 then purified by gel permeation chromatography(GPC) or solid phase extraction(SPE). The recoveries ranged from 70.1% to 95.7% with the cleaning method of GPC and from 70.2% to 94.9% with the cleaning method of primarysecondary amine PSA SPE. The limits of detection(LOD) were 1×10-5 g/kg. The method showed a good linear relationship with the correlation coefficients over 0.99.This method is practical, accurate and highly sensitive.

Key words: UPLC-MS/MS, vegetable, mushroon, carbamate

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