液相色谱-串联质谱法同时检测蔬菜中克百威和3-羟基克百威残留.pdf

第8卷第4期
食品安全质量检测学报
Vol. 8 No 4
2017年4月
Journal of Food Safety and Quality
Apr,2017
液相色谱-串联质谱法同时检测蔬萊中克百威和
3-羟基克百威残留
姚丽君',杨路2,代弟2,王秋艳2,徐静2,曹际娟2”
营口市食品安全检验检测中心,营口1150002.辽宁出入境检验检疫局,大连100083
摘要:目的建立一种克百威及3-羟基克百威衣药残留的液相色谱-串联质谱( liquid chromatography
tandem mass spectrometry,LC-MS/AMS)检测方法。方法样品经乙腈提取,氯化钠盐析除水后,过氨基固相萃
取柱净化,甲醇和二氯甲烷混合溶液洗脱。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,
质谱(ESI+)采用多离子检测模式(MRM)对定量离子和定性离子进行监测。结果本方法在15min内完成2种
目标化合物的分离分析。克百威和3-羟基克百威在10、30和100?gkg添加水平的回收率为72.09%~106.4%,相
对标准偏差小于6.9%(n=60,方法定量限为10ugkg。结论该方法快速、准确、灵敏,适合测定蔬菜中克百
威及3-羟基克百威药物残留。
关键词:克百威;3-羟基克百威;液相色谱-串联质谱法;农药残留
Simultaneous determination of carbofuran and 3-hydroxycarbofuran
residues in vegetables by liquid chromatography-tandem mass spectrometry
YAO Li-jun YANG Lu, DAI Di, WANG Qiu-yan, XU Jing, CAO Ji-juan
(1. Yingkou Food Safety Inspection and Testing Center, Yingkou 115000, China; 2. Liaoning Entry-exit Inspection
and Quarantine Bureau, Dalian 100083, China
ABSTRACT: Objective To establish a method for Simultaneous determination of carbofuran and
3-hydroxycarbofuran residues in vegetable samples by liquid chromatography-tandem mass spectrometric
(LC-MS/MS). Methods Vegetable samples were extracted with acetonitrile, and water was removed after saltin
out by sodium chloride. And then carbofuran and 3-hydroxycarbofuran residues in the extracts were separated on an
amino solid phase extraction column using a gradient elution program of 0.1% formic acid aqueous solution(A) and
0.1% formic acid in acetonitrile solution(B). Using LC-MS/MS(ESI)with multiple reactions monitoring(MRM)
identification of the major components of the residues was performed based upon the intensities of fragments
Results The established method could separate and analyze the two target compounds within 15 min. The
recoveries were ranged from 72.0% to 106.4% for the 2 residues with 3 spiked levels of 10, 30 and 100 ug/kg. The
relative standard deviations( RSDS )were less than 6. 9%(n=6), and the limits of quantitation(LOQ)for the 2 residues
were 10 ug/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting
基金项目;国家质检总局科技项目(2014K113
Fund: Supported by the Science Foundation of Inspection and Quarantine of the Peoples Republic of China(2014IK113)
通讯作者:徐静,高级工程师,主要研究方向为食品安全。E-mai:Jingxu99@163.com
曹际娟,研究员,主要研究方向为食品安全。E-mail:caojj(0909163.com
Corresponding author: XU Jing, Senior Engin, oning Eny-exit Inson and Quaanne Buea Dalian 100083, China E-mail inu 163. m
CA, Professor Liaoning En -it I on and Quarantine au Dalian 100083, China E mail caoi 163. m
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