固相萃取UPLC-MS/MS法同时检测鸡肉中8种抗病毒药物的残留量  

Simultaneous determination of eight antiviral drugs residues in chicken by solid-phase extraction combined with UPLC-MS/MS

作　　者：杨旭[1] 刘正才[2] 杨方[2] 林永辉[2] 苏芝娇[2] 姚闽娜[1] 

机构地区：[1]福建农林大学食品科学学院,福州350002 [2]福建出入境检验检疫局福建省检验检疫技术研究重点实验室,福州350001

出　　处：《药物分析杂志》2016年第3期513-521,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家质检总局科技项目(2014IK110);福建省科技重点项目(k5312001;2012Y6001)资助项目

摘　　要：目的:建立了鸡肉中8种抗病毒药物(阿昔洛韦、扎那米韦、拉米夫定、阿比朵尔、奥司他韦、咪喹莫特、金刚烷胺、金刚乙胺)残留量的固相萃取-超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法:样品用0.2 mol·L^(-1)盐酸溶液-乙腈(9∶1)超声提取,上清液经MCX固相萃取柱净化,采用GP-C8(100 mm×3.0 mm,3μm)柱以0.2%甲酸溶液-乙腈为流动相梯度洗脱分离,电喷雾电离(ESI)正离子多反应监测模式(MRM)进行测定,内标法定量。结果:阿昔洛韦、扎那米韦、拉米夫定、阿比朵尔、奥司他韦、咪喹莫特、金刚烷胺、金刚乙胺质量浓度在1~20 ng·mL^(-1)范围内线性关系良好,相关系数R2均大于0.990;方法的检出限(LOD)为0.6~1.0μg·kg^(-1),定量限(LOQ)为2.0~3.4μg·kg^(-1)。鸡肉中在2.0、5.0、20.0μg·kg^(-1) 3个加标水平的平均回收率为76.4%~95.7%,RSD为4.5%~11.7%;该方法应用于实际鸡肉样品的检测分析,其中2份检出金刚烷胺残留,其他化合物均未检出。结论:本法经方法学验证,可用于鸡肉中阿昔洛韦、扎那米韦、拉米夫定、阿比朵尔、奥司他韦、咪喹莫特、金刚烷胺、金刚乙胺残留量的的确证检测。Objective：To develop a method for the determination of antivirals（acyclovir,zanamivir,lamivudine,arbidol,oseltamivir,imiquimod,amantadine,rimantadine）in chicken by solid-phase extraction combined with ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.Methods：After ultrasonically extracted by（0.2 mol·L-（-1））hydrochloric acid-acetonitrile（9 ∶ 1）and purified by a MCX SPE cartridge,the samples were loaded onto GP-C8 column（100 mm×3.0 mm,3 μm）using a mobile phase consisting of 0.2% formic acid（volume fraction）and acetonitrile.The electrospray ionization（ESI）source in the positive mode and the multiple-reaction monitoring（MRM）mode were used for the quantitative analysis with internal standard.Results：The results showed that the calibration curves were in good linearity for the antivirals ranged from 1 to 20 ng·m L-（-1） with the correlation coefficients（R2）above 0.990.The limits of detection（LODs）and the limits of quantification（LOQs）of this method were 0.6-（-1）.0 μg·kg-（-1） and 2.0-3.4 μg·kg-（-1） for the eight analytes,respectively.The average recovery rates were from 76.4% to 95.7% with the relative standard deviations（RSDs）from 4.5% to11.7% at three standard addition levels of 2.0 μg·kg-（-1）,5.0 μg·kg-（-1）,and 20.0 μg·kg-（-1）.By this method applied for the determination of residues of antiviral drugs in real chickens,amantadine was detected in two samples,and other compounds were not detected.Conclusion：The method is simple,accurate,rapid,sensitive,which can be adopted for simultaneous confirmation of residues of eight antivirals in chicken.

关 键 词：食品安全监测 药物残留量 抗病毒药物 阿昔洛韦 扎那米韦 拉米夫定 阿比朵尔 奥司他韦 咪喹莫特 金刚烷胺 金刚乙胺 超高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]