色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 954-960.DOI: 10.3724/SP.J.1123.2013.04028

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定蔬菜和水果中6种新型酰胺类杀菌剂的残留量

陈小龙, 李正翔, 曹赵云, 巩佳第, 曹晓林, 陈铭学   

  1. 中国水稻研究所, 农业部稻米及制品质量监督检验测试中心, 浙江 杭州 310006
  • 收稿日期:2013-04-17 修回日期:2013-05-31 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 陈铭学
  • 基金资助:

    浙江省级重点科技创新团队项目(2012R10028-05).

Determination of six novel amide fungicides in vegetables and fruits by liquid chromatography-tandem mass spectrometry

CHEN Xiaolong, LI Zhengxiang, CAO Zhaoyun, GONG Jiadi, CAO Xiaolin, CHEN Mingxue   

  1. Rice Product Quality Inspection and Supervision Center of Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China
  • Received:2013-04-17 Revised:2013-05-31 Online:2013-10-28 Published:2013-10-08

PDF

366

被引次数

22

摘要：

建立了蔬菜、水果中啶酰菌胺、氟啶酰菌胺、环氟菌胺、嘧菌胺、双炔酰菌胺和硅噻菌胺6种新型酰胺类杀菌剂残留量的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测方法。试样经乙腈提取、Florisil固相萃取柱净化、以乙腈和水为流动相梯度洗脱、结合新型核壳型填料色谱柱(Poroshell 120 EC-C18)分离,采用电喷雾正离子扫描、多反应监测模式质谱检测,外标法定量。结果表明:固相萃取结合新型色谱柱分离解决了酰胺类农药分析中基质效应强的难点问题。6种杀菌剂在0.5~100 μg/L范围内线性关系良好,相关系数(r)≥0.9990;对7种蔬菜及3种水果进行0.5、5和50 μg/kg 3个加标水平的回收试验,回收率为65%~124%,相对标准偏差(RSD, n=5)为1%~18%; 6种杀菌剂的方法检出限(S/N≥3)为0.10~0.17 μg/kg。该净化、分离模式显著降低了蔬菜、水果中6种新型酰胺类农药的基质效应,方法简单准确,可满足蔬菜和水果中啶酰菌胺等6种新型酰胺类杀菌剂残留检测的要求。

关键词: 蔬菜, 水果, 酰胺类杀菌剂, 液相色谱-串联质谱

Abstract:

A method was developed for the simultaneous determination of mepanipyrim, silthiofam, boscalid, fluopicolide, mandipropamid, cyflufenamid in vegetables and fruits by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted from the samples by acetonitrile and purified by Florisil SPE. The six novel amide fungicides were separated on a Poroshell 120 EC-C18 column with the mobile phases of water and acetonitrile, and finally detected by MS/MS with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, quantified by external standard method. Under the optimal analytical conditions, the correlation coefficients (r) of the six novel amide fungicides were not lower than 0.9990 in the concentration range from 0.5 to 100 μg/L. The limits of detection (S/N≥3) of the method were 0.15 μg/kg for boscalid, silthiofam, mandipropamid, cyflufenamid, 0.10 μg/kg for mepanipyrim and 0.17 μg/kg for fluopicolide. The recovery tests were performed for the 7 types of vegetables and the 3 types of fruits at the spiked levels of 0.5, 5 and 50 μg/kg, and the recoveries of the six analytes ranged from 65% to 124% with the relative standard deviations (RSDs, n=5) of 1%-18%. The matrix effects in vegetables and fruits of the six amide fungicides were significantly reduced by the purification of Florisil SPE compared with the modified QuEChERS. The method is easy, fast, sensitive and accurate, and can meet the requirements of the determination of the six amide fungicide residues in vegetables and fruits.

Key words: amide fungicides, fruits, liquid chromatography-tandem mass spectrometry (LC-MS/MS), vegetables

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