快速滤过型净化法结合气相色谱-四极杆-飞行时间质谱同时筛查果蔬中234种农药残留被引量：19

Rapid Screening of 234 Pesticide Residues in Vegetables and Fruits by Multi-plug Filtration Cleanup Method Combined with Gas Chromatography-Quadrupole Time of Flight Mass Spectrometry

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摘要建立快速滤过型净化法结合气相色谱-四极杆-飞行时间质谱同时筛查蔬菜和水果中234种农药残留的方法。样品经过乙腈提取,提取液用m-PFC柱净化后,经气相色谱-四极杆-飞行时间质谱仪测定。通过保留时间和全扫描离子精确质量数定性,基质标准曲线定量,能够有效去除基质干扰。对12种典型果蔬样品(白菜、芹菜、番茄、黄瓜、菠菜、韭菜、油菜、橘子、梨、苹果、葡萄、橙子)进行实际样品验证。结果表明,234种农药在5~500μg/kg范围内线性良好,相关系数大于0.990,方法的检出限为5~20.0μg/kg。样品在10、50、100μg/kg 3个添加水平的平均加标回收率分别为73.2%~124.8%、75.5%~122.6%和74.8%~121.7%,平均相对标准偏差分别为2.4%~13.2%、2.8%~11.4%和2.2%~10.5%。该方法有效地提高了高分辨质谱在进行果蔬农药高通量筛查时的检测效率,具有较强的实际应用价值。 A new method for screening pesticide residues in vegetables and fruits by multi-plug filtration cleanup(m-PFC)method combined with gas chromatography-quadrupole time of flight mass spectrometry(GC-QTOF-MS)was developed.The samples were extracted with acetonitrile,purified by m-PFC,and detected by GC-QTOF-MS.Qualitative analysis was carried out by retention time and accurate mass measurements in full scan mode and quantitation was performed using matrix-matched standard calibration,which could effectively eliminate matrix interference.Twelve typical samples(Chinese cabbage,celery,tomato,cucumber,spinach,Chinese leek,pakchoi,tangerine,pear,apple,grape,and orange)were used to evaluate the method.Good linearity was achieved for 234 pesticides in the concentration range of 5 to 500μg/kg with correlation coefficients greater than 0.990.The results showed that the limits of detection of this method were in the range of 5–20μg/kg.The average recoveries at three spiked levels of 10,50,and 100μg/kg were in the range of 73.2%–124.8%,75.5%–122.6%and 74.8%–121.7%,with relative standard deviations(RSDs)of 2.4%–13.2%,2.8%–11.4%and 2.2%–10.5%,respectively.The method could effectively improve the detection efficiency of high-resolution mass spectrometry for high throughput screening of pesticide residues in vegetables and fruits,thereby having great potential for practical application.

作者孟志娟黄云霞邸鹏月赵丽敏牛立沙范素芳李强张岩 MENG Zhijuan;HUANG Yunxia;DI Pengyue;ZHAO Limin;NIU Lisha;FAN Sufang;LI Qiang;ZHANG Yan(Key Laboratory of Food Safety of Hebei Province,Hebei Food Inspection and Research Institute,Shijiazhuang 050091,China)

机构地区河北省食品检验研究院河北省食品安全重点实验室

出处《食品科学》 EI CAS CSCD 北大核心 2020年第16期272-285,共14页 Food Science

基金 “十三五”国家重点研发计划重点专项(2018YFC1603400) 河北省科技计划项目(19225503D) 国家市场监管总局技术保障专项(2019YJ009) 河北省市场监督管理局科研计划项目(2020ZC06)。

关键词气相色谱-四极杆-飞行时间质谱快速滤过型净化农药残留快速筛查果蔬 gas chromatography-quadrupole time of flight mass spectrometry multi-plug filtration cleanup pesticide residues rapid screening vegetables and fruits

分类号 O657.63 [理学—分析化学]