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QuEChERS-UPLC-MS/MS测定果蔬中18种琥珀酸脱氢酶抑制剂类杀菌剂

龚蕾   

  1. 湖北省食品质量安全监督检验研究院
  • 收稿日期:2020-05-28 修回日期:2021-04-27 出版日期:2021-09-25 发布日期:2021-09-24
  • 通讯作者: 龚蕾 E-mail:gonglei406@163.com
  • 基金资助:
    国家重点研发计划

Determination of 18 succinate dehydrogenase inhibitors( SDHIs) fungicides in foods by ultra-performance liquid chromatography-tandem mass spectrometer

Lei GONG   

  • Received:2020-05-28 Revised:2021-04-27 Online:2021-09-25 Published:2021-09-24
  • Contact: Lei GONG E-mail:gonglei406@163.com

摘要: 摘 要:建立改进的QuEChERS提取和净化方法,结合超高效液相色谱串联质谱法(UPLC-MS/MS)测定果蔬中18种琥珀酸脱氢酶抑制剂类杀菌剂。样品经乙腈均质提取,无水硫酸镁及醋酸钠脱水盐析,乙二胺?N?丙基硅烷(PSA)净化,以乙腈?0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,采用正负离子同时扫描,多反应监测(MRM)模式,使18种目标化合物在C18色谱柱上分离,外标法定量。18种目标化合物在0.5~200 μg/L范围内线性关系良好,相关系数均大于0.99,方法检出限为0.5~2.0 μg/kg,定量限为1.5~6.0 μg/kg。各种目标化合物在4种基质中3个添加水平(10、50和150 μg/kg)下的回收率为83.6%~109.4%,相对标准偏差(RSD,n=6)为1.2%~8.4%。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: 超高效液相色谱?串联质谱, QuEChERS, 琥珀酸脱氢酶抑制剂类杀菌剂, 果蔬

Abstract: Abstract: :A modified QuEChERS coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 18 succinate dehydrogenase inhibitors( SDHIs) fungicides in fruits and vegetables. Samples were extracted with acetonitrile and salted out with anhydrous magnesium sulfate and sodium acetate, then purified by primary secondary amine(PSA). The eighteen compounds were separated on a C18 column by the gradient elution using acetonitrile-0.1%(V/V) formic acid aqueous solution as mobile phase, detected by MS/MS with both positive and negative mode in multiple reaction monitoring (MRM) mode, and finally quanitified by external standard method. The correlation coeffcients(r) of the eighteen compounds were above 0.99 in the concentration ranging from 0.5~200 μg/L. The limits of detection and the limits of quantification of the method were 0.5~2.0 μg/kg and 1.5~6.0 μg/kg, respectively. The recoveries spiked at three levels(10, 50 and 150 μg/kg) in four different matrices ranged from 83.6% to109.4% with the relative standard deviations (RSDs, n=6). The method is easy to operate and with good purification effect. It can be applied to the rapid determination of the SDHIs in fruits and vegetables.

Key words: ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), QuEChERS, succinate dehydropgenase inhibitor( SDHI) fungicides, fruits and vegetables

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