食品科学 ›› 2021, Vol. 42 ›› Issue (18): 261-268.doi: 10.7506/spkx1002-6630-20200528-345

• 安全检测 • 上一篇    下一篇

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,黄徽,韩智,江丰,彭青枝,黄宗骞,王亨   

  1. (湖北省食品质量安全监督检验研究院,湖北省食品质量安全检测工程技术研究中心,湖北 武汉 430070)
  • 发布日期:2021-09-29
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1602303)

Determination of 18 Succinate Dehydrogenase Inhibitor Fungicides in Foods by Modified QuEChERS Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

GONG Lei, HUANG Hui, HAN Zhi, JIANG Feng, PENG Qingzhi, HUANG Zongqian, WANG Heng   

  1. (Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Provincial Institute for Food Supervision and Test, Wuhan 430070, China)
  • Published:2021-09-29

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(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法测定果蔬中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-丙基硅烷净化,以乙腈-0.1%甲酸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 μg/kg和150 μg/kg)下的回收率为83.6%~109.4%,相对标准偏差为1.2%~8.4%(n=6)。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: A modified QuEChERS coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 18 succinate dehydrogenase inhibitor (SDHI) fungicides in fruits and vegetables. Samples were extracted with acetonitrile and salted out with anhydrous magnesium sulfate and sodium acetate, and then the supernatant was purified with primary secondary amine (PSA). The 18 compounds were separated on a C18 column by gradient elution using acetonitrile-0.1% (V/V) formic acid in water as the mobile phase, detected by MS/MS in both positive ion and negative ion mode using multiple reaction monitoring (MRM), and finally quantified by the external standard method. The calibration curves for all analytes showed good linearity with correlation coefficients (r) of above 0.99 in the concentration range of 0.5–200 μg/L. The limits of detection (LOD) and the limits of quantification (LOQ) of the developed method were 0.5–2.0 and 1.5–6.0 μg/kg, respectively. The recoveries of the analytes in four different matrixes each spiked at three levels (10, 50 and 150 μg/kg) ranged from 83.6% to 109.4% with relative standard deviations (RSD) of 1.2%–8.4% (n = 6). This method was easy to operate and showed good purification efficiency, and thus it could be applied to the rapid determination of SDHI fungicides in fruits and vegetables.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; quick, easy, cheap, effective, rugged and safe; succinate dehydropgenase inhibitor fungicides; fruits and vegetables

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