摘要
建立了动物源性食品中15种抗病毒类药物残留的通过式净化-亲水作用色谱-串联质谱分析方法。样品经1%酸化乙腈溶液超声提取,冷冻离心后,经PRi ME HLB小柱净化,直接进样分析。以资生堂PC HILIC色谱柱进行分离,以10 mmol/L乙酸铵(含0.2%甲酸)和乙腈为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离、多反应监测(MRM)模式进行检测,基质匹配标准工作曲线定量。结果表明,15种抗病毒药物在0.2~80μg/kg范围内呈良好线性关系,相关系数(r^(2))均大于0.999,15种抗病毒药物的检出限为0.1~1.0μg/kg之间,0.3,5.0,20μg/kg 3水平的加标回收率在65.9%~115%之间,RSDs为1.7%~9.2%。
A method for detecting 15 kinds of anti-viral drug residues in animal-derived foods was established by passing purification-ultra-performance hydrophilic interaction chromatography-tandem mass spectrometry.The samples were first extracted by 1%acetic acid-acetonitrile solution,then purified by PRi ME HLB column.The15 kinds of anti-viral drugs were separated by PC HILIC column(2.0 mm×100 mm,3μm)and gradiently eluted using acetonitrile and 10 mmol/L ammonium acetate solution(containing 0.2%formic acid)as moble phase.The detection of anti-viral drugs was performed by tandem mass spectrometry in electrospray ionization under multiple reactions monitoring(MRM)mode.The calibration curves for target compounds were linear over the range of 0.2-80μg/kg with correlation coefficients(r^(2))larger than 0.999.The recoveries of the 15 kinds of anti-viral drugs at three spiked levels were between 65.9%and 115%with the relative standard deviations of1.7%-9.2%.The detection limits of the 15 kinds of anti-viral drugs ranged from 0.1 to 1.0μg/kg.
作者
叶佳明
杨娜
王京
钟世欢
叶磊海
裘钧陶
陈青俊
YE Jiaming;YANG Na;WANG Jing;ZHONG Shihuan;YE Leihai;QIU Juntao;CHEN Qingjun(Zhejiang Gongzheng Testing Center,Co.,Ltd.,Hangzhou 310009;Zanyu Technology Group Co.,Ltd.,Hangzhou 310009)
出处
《分析试验室》
CAS
CSCD
北大核心
2021年第4期462-468,共7页
Chinese Journal of Analysis Laboratory
基金
浙江省基础公益研究计划项目(LGN19B050003)资助。
