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

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^-13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, 3μm) 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·mL^-1 with the correlation coefficients(R²) above 0.990.The limits of detection(LODs) and the limits of quantification(LOQs) of this method were 0.6-1.0μg·kg^-1 and 2.0-3.4μg·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 2.0μg·kg^-1, 5.0μg·kg^-1, and 20.0μg·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.