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食品与发酵工业  2022, Vol. 48 Issue (20): 231-237    DOI: 10.13995/j.cnki.11-1802/ts.029826
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
超高效液相色谱-串联四级杆质谱联用法测定14种蔬菜中灭蝇胺的残留
俞所银1, 闫晴1, 梁佳2,3*
1(上海市质量技术监督检验技术研究院,上海,200233)
2(浙江海洋大学 食品与药学学院,浙江 舟山,316022)
3(浙江省海产品健康危害因素关键技术研究重点实验室,浙江 舟山,316021)
Determination of cyromazine residues in 14 kinds of vegetables by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS)
YU Suoyin1, YAN Qing1, LIANG Jia2,3*
1(Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200233, China)
2(College of Food Sciences and Pharmaceutics, Zhejiang Ocean University, Zhoushan 316022, China)
3(Zhejiang Provincial Key Laboratory of Health Risk Factors for Seafood, Collaborative Innovation Center of Seafood Deep Processing, Zhoushan 316021, China)
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摘要 建立了韭菜等14种蔬菜中灭蝇胺残留量的超高效液相色谱-串联四级杆质谱联用法(ultra-high performance liquid chromatography-triple quadrupole mass spectrometry, UPLC-QQQMS)测定方法。样品采用乙腈提取、取5 mL上清液氮吹干,1 mL乙腈定容。亲水作用HILIC柱分离,以含0.1%甲酸的5 mmol/L乙酸铵溶液和乙腈作为流动相等度洗脱,正离子电喷雾(electron spray ionization, ESI+)电离扫描、多反应监测(multiple reaction monitoring, MRM)模式,基质标准曲线外标法定量。灭蝇胺在0.5~100 μg/L均有较好的线性关系(r>0.99),在2.0、4.0、20.0 μg/kg 3个添加水平下,14种蔬菜中灭蝇胺回收率均在80%~113%,相对标准偏差为0.56%~7.21%,检出限(S/N=3)为0.5 μg/kg,方法定量限(S/N=10)均为2.0 μg/kg。
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俞所银
闫晴
梁佳
关键词:  基质标准  超高效液相色谱-串联四级杆质谱联用法  蔬菜  灭蝇胺  农药残留    
Abstract: A method for the determination of cyromazine residues in 14 kinds of vegetables including garlic chives by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS) was established. The samples were extracted with acetonitrile, and then 5 mL supernatant liquid was evaporated with a nitrogen stream and dissolved in 1 mL acetonitrile. The dissolving solution was separated with a hydrophilic chromatography column by isocratic elution using 5 mmol/L ammonium acetate solution containing 0.1% formic acid with acetonitrile as mobile phases. Then, it was detected by electrospray ion source positive ion detection mode and multiple reaction monitoring modes, and quantified by the matrix-matched external standard calibration curves. Cyromazine had a good linear relationship in the concentration range of 0.5-100 μg/L with good correlation coefficients (r>0.99). The average recoveries ranged from 80% to 113% for cyromazine at 3 spiked levels of 2.0, 4.0, and 20.0 μg/kg. The relative standard deviations (RSD, n=3) were in the range of 0.56%-7.21%. The limits of detection were 0.5 μg/kg (S/N=3) and the limits of quantification detection were 2.0 μg/kg(S/N=10).
Key words:  matrix-matched external standard calibration curves    ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS)    vegetables    cyromazine    pesticide residues
收稿日期:  2021-10-26      修回日期:  2021-12-16           出版日期:  2022-10-25      发布日期:  2022-11-18      期的出版日期:  2022-10-25
基金资助: 国家重点研发计划课题食品安全快检智能化移动终端与取证快速筛查技术应用示范研究(2019YFC1606404)
作者简介:  硕士,工程师(梁佳讲师为通信作者,E-mail:liangjia@zjou.edu.cn)
引用本文:    
俞所银,闫晴,梁佳. 超高效液相色谱-串联四级杆质谱联用法测定14种蔬菜中灭蝇胺的残留[J]. 食品与发酵工业, 2022, 48(20): 231-237.
俞所银,闫晴,梁佳. Determination of cyromazine residues in 14 kinds of vegetables by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS)[J]. Food and Fermentation Industries, 2022, 48(20): 231-237.
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http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.029826  或          http://sf1970.cnif.cn/CN/Y2022/V48/I20/231
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