色谱

色谱 ›› 2016, Vol. 34 ›› Issue (11): 1070-1076.DOI: 10.3724/SP.J.1123.2016.07005

• 研究论文 • 上一篇    下一篇

改良QuEChERS方法快速测定果蔬中8种新型琥珀酸脱氢酶抑制剂类杀菌剂

杨欢, 孙伟华, 曹赵云, 马有宁, 柴爽爽, 秦美玲, 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, 农业部稻米产品质量安全风险评估实验室, 浙江 杭州 310006
  • 收稿日期:2016-07-04 出版日期:2016-11-08 发布日期:2016-11-03
  • 通讯作者: 陈铭学
  • 基金资助:

    国家农产品质量安全风险评估项目（GJFP2016001001）；中央级公益性科研院所基本科研业务费专项资金项目（2014RG006）.

Determination of eight novel succinate dehydrogenase inhibitor fungicides in vegetables and fruits by modified QuEChERS

YANG Huan, SUN Weihua, CAO Zhaoyun, MA Youning, CHAI Shuangshuang, QIN Meiling, CHEN Mingxue   

  1. Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Rice, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China
  • Received:2016-07-04 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    National Agricultural Product Quality Safety Risk Assessment Project (No. GJFP2016001001); Central Public Welfare Scientific Research Basic Business Expenses Special Funds for Scientific Research Projects (No. 2014RG006).

PDF

170

被引次数

8

摘要：

建立了一种同时测定果蔬中啶酰菌胺、吡噻菌胺、吡唑萘菌胺、氟唑菌酰胺、联苯吡菌胺、氟唑环菌胺、氟唑菌苯胺和氟吡菌酰胺8种新型琥珀酸脱氢酶抑制剂类杀菌剂残留量的液相色谱-串联质谱方法。通过比较乙二胺-N-丙基硅烷（PSA）和十八烷基键合硅胶吸附剂（C18）两种分散固相萃取剂不同添加剂量下的吸附作用和净化效果，优化QuEChERS方法净化过程，以乙腈-0.1%（体积分数）甲酸水溶液为流动相进行梯度洗脱，使8种目标化合物在Poroshell 120 EC-C18色谱柱上分离，经电喷雾正/负双离子扫描、多反应监测模式质谱检测，外标法定量。8种目标化合物在0.5~500.0 μg/L范围内线性关系良好，相关系数均大于0.998，方法检出限为0.2~1.7 μg/kg，定量限为0.5~5.0 μg/kg。各种目标化合物在8种基质中3个添加水平（5.0、25.0和125.0 μg/kg）下的回收率为71.4%~121.3%，相对标准偏差（RSD，n=6）为0.8%~17.2%。该方法操作简单、净化效果好，适用于果蔬中新型琥珀酸脱氢酶抑制剂类杀菌剂的快速检测。

关键词: QuEChERS, 蔬菜, 水果, 新型琥珀酸脱氢酶抑制剂类杀菌剂, 液相色谱-串联质谱

Abstract:

A method was developed for the simultaneous determination of eight novel succinate dehydrogenase inhibitor fungicides (boscalid, penflufen, bixafen, sedaxane, fluopyram, penthiopyrad, isopyrazam, fluxapyroxad) residues in vegetables and fruits by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with modified QuEChERS. The amount of the two solid phase extraction agents (octadecyl bonded silica (C18) and primary secondary amine (PSA)) in QuEChERS method was optimized according to their adsorption and purification capacities. The eight compounds were extracted from samples by acetonitrile and purified by solid phase extraction agents. The eight compounds were separated on a Poroshell 120 EC-C18 column by the gradient elution using acetonitrile-0.1% (v/v) formic acid aqueous solution as mobile phases, detected by MS/MS with positive/negative electrospray ionization (ESI+/ESI-) in multiple reaction monitoring (MRM) mode, and finally quantified by external standard method. The correlation coeffcients (r) of the eight compounds were all above 0.998 in the mass concentration ranging from 0.5 to 500.0 μg/L. The limits of detection and the limits of quantification of the method were 0.2-1.7 μg/kg and 0.5-5.0 μg/kg, respectively. The recoveries of the eight analytes spiked at three levels (5.0, 25.0 and 125.0 μg/kg) in eight matrices ranged from 71.4% to 121.3% with the relative standard deviations (RSDs, n=6) from 0.8% to 17.2%. The method is easy to operate and with good purification effect. It can be applied to the rapid determination of the novel succinate dehydrogenase inhibitor fungicides in vegetables and fruits.

Key words: fruits, liquid chromatography-tandem mass spectrometry (LC-MS/MS), novel succinate dehydrogenase inhibitor (SDHI) fungicides, QuEChERS, vegetables

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