液相色谱-串联质谱法同时测定鸡蛋中4种抗病毒药物残留  

Simultaneous determination of four antiviral drug residues in eggs by liquid chromatography-tandem mass spectrometry

作　　者：孙玲玲 霍江莲[3] 陈冬东[1] 呼秀智 霍思宇 耿旭浩 高家政 彭涛[1] 薛占永 SUN Lingling;HUO Jianglian;CHEN Dongdong;HU Xiuzhi;HUO Siyu;GENG Xuhao;GAO Jiazheng;PENG Tao;XUE Zhanyong(Chinese Academy of Inspection and Quarantine,Beijing,100176,China;School of Life Science and Food Engineering,Hebei University of Engineering;China National Accreditation Center for Conformity Assessment;Cas(Beijing)Science and Technology Co.,Ltd.)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]河北工程大学生命科学与食品工程学院 [3]中国合格评定国家认可中心 [4]检科院(北京)科学技术有限公司

出　　处：《质量安全与检验检测》2023年第5期6-13,30,共9页QUALITY SAFETY INSPECTION AND TESTING

基　　金：现场执法快检产品多维评价技术研究与认证应用(2022YFF1101004)。

摘　　要：建立液相色谱-串联质谱法同时测定鸡蛋样品中4种抗病毒药物(金刚烷胺、金刚乙胺、利巴韦林和吗啉胍)残留量的分析方法。鸡蛋样品残留的目标物质通过1%甲酸乙腈提取,经MgSO4、N-丙基乙二胺(primary secondary amine,PSA)、十八烷基硅胶C18和石墨化炭黑(graphitized carbon black,GCB)分散固相萃取净化,40℃水浴中氮气吹干后复溶。采用色谱柱Shim-pack Velox HILIC(2.1×150 mm,2.7μm),流动相A为乙腈,B为20 mM甲酸铵+0.1%甲酸溶液,进行梯度洗脱,4种目标物质正离子模式监测,内标法定量进行分析。结果显示,4种抗病毒药物在一定浓度范围内线性良好,相关系数(R2)均大于0.9960,检出限在0.1~1.5μg/kg范围之间,定量限在0.3~4.0μg/kg范围之间。4种药物在各自定量限1、1.5、2倍添加浓度水平下添加回收率在75.9%~110.1%之间,相对标准偏差(relative standard deviations,RSDs)为3.2%~6.9%。该方法操作简单、灵敏度高、回收率好,可用于日常鸡蛋样品中抗病毒类药物的残留检测。A method for simultaneous determination of amantadine,amantadine,ribavirin and morpholine guanidine residues in eggs by liquid chromatography-tandem mass spectrometry was established.The residual target substance in the egg sample was extracted with 1%formic acid acetonitrile,then purified by MgSO_(4),primary secondary amine(PSA),octadecyl silica gel C18 and graphitized carbon black(GCB)by solid phase extraction,dried in a water bath at 40℃and then dissolved again.Chromatographic column Shim-pack Velox HILIC(2.1×150 mm,2.7μm),mobile phase A is acetonitrile,B is 20 mM ammonium formate+0.1%formic acid solution,gradient elution,positive ion mode monitoring of four target substances,quantitative internal standard method.The results showed that the four antiviral drugs were linear in a certain concentration range,the correlation coefficients(R2)were all more than 0.9960,the detection limits were in the range of 0.1-1.5μg/kg,and the quantitative limits were in the range of 0.3-4.0μg/kg.The recovery of the four drugs was between 75.9%and 110.1%,and the relative standard deviations(RSDs)was 3.2%and 6.9%at the respective quantitative limits of 1,1.5,2 times the concentration level.The method has the advantages of simple operation,high sensitivity and good recovery,and can be used for the residue detection of antiviral drugs in daily egg samples.

关 键 词：鸡蛋 抗病毒类药物 分散固相萃取 液相色谱-串联质谱法 残留 

分 类 号：S859.84[农业科学—临床兽医学]