摘要
建立固相萃取(SPE)–气相色谱–三重四级杆质谱(GC–MS–MS)法检测禽蛋及蛋制品中氟虫腈残留量的分析方法。样品采用乙腈提取,经固相萃取小柱净化,GC–MS–MS检测,基质匹配外标法定量。氟虫腈的质量浓度在0.01～0.10 mg/L范围内与色谱峰面积呈良好的线性关系,相关系数r大于0.999,方法的定量限(10S/N)为0.001 mg/kg。在0.01,0.02,0.10 mg/kg 3种浓度添加水平下,平均回收率为86.7%～109.8%,测定结果的相对标准偏差为4.8%～9.9%(n=6)。该方法准确、灵敏、简单、高效,适合禽蛋及蛋制品中氟虫腈残留的定性定量分析。
A method for the determination of fipronil residues in eggs and egg products by solid phase extraction–gas chromatography–triple quadrupole tandem mass spectrometry(GC–MS–MS)was established.The residues in the samples were extracted with aqueous solution,then cleaned up by solid phase extraction column and determined by GC–MS–MS.Matrix matched and external standard method was used for quantitative.The mass concentration of fipronil had good linear relationship with the chromatographic peak area in the range of 0.01–0.10 mg/L,and the linear correlation coefficient was more than 0.999,the limit of quantification(10S/N)was 0.001 mg/kg.At the spiked concentrations of 0.01,0.02,0.10 mg/kg,the average recoveries were ranged from 86.7%to 109.8%,the relative standard deviation of determination results was 4.8%–9.9%(n=6).The method has the advantage of high accuracy and sensitivity,simple and effective,which is suitable for the qualitative and quantitative determination of fipronil residues in egg and egg product.
作者
蒲云月
陈少波
PU Yunyue;CHEN Shaobo(Suzhou Inspection and Quarantine Technical Center,Suzhou 215104,China;Suzhou World Standard Testing Technology Co.,Ltd.,Suzhou 215104,China;Suzhou Huabo Daily Chemicals Testing&Service Co.,Ltd.,Suzhou 215104,China)
出处
《化学分析计量》
CAS
2018年第5期80-83,共4页
Chemical Analysis And Meterage
关键词
氟虫腈
气相色谱–三重四级杆质谱法
禽蛋及蛋制品
fipronil
gas chromatography–triple quadrupole tandem mass spectrometry
egg and egg product
