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
目的 建立一种克百威及3-羟基克百威农药残留的液相色谱-串联质谱(liquid chromatography- tandem mass spectrometry, LC-MS/MS)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15 min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 μg/kg添加水平的回收率为72.0%~106.4%, 相对标准偏差小于6.9%(n=6), 方法定量限为10 μg/kg。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。
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 salting 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 μg/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 μg/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting carbofuran and 3-hydroxycarbofuran residues in vegetable samples.
标题：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
英文标题：Simultaneous determination of carbofuran and 3-hydroxycarbofuran residues in vegetables by liquid chromatography-tandem mass spectrometry
作者：
姚丽君 营口市食品安全检验检测中心
杨璐 辽宁出入境检验检疫局
代弟 辽宁出入境检验检疫局
王秋艳 辽宁出入境检验检疫局
徐静 辽宁出入境检验检疫局
曹际娟 辽宁出入境检验检疫局
中文关键词:克百威,3-羟基克百威,液相色谱-串联质谱法,农药残留,
英文关键词:carbofuran,3-hydroxycarbofuran,liquid chromatography-tandem mass spectrometry,pesticide residues,
发表日期：2017-03-03
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