超高效液相色谱-串联质谱法测定鸡组织中利巴韦林的残留量及其前处理方法优化  

Optimization of sample pretreatment and determination of ribavirin residues in chicken tissues by ultraperformance liquid chromatography-tandem mass spectrometry

作　　者：刘正才[1] 杨方[1] 徐姗[2] 林永辉[1] 苏芝娇[1] 潘迎芬[1] 杨旭[3] 

机构地区：[1]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 [2]北京出入境检验检疫局检验检疫技术中心,北京100026 [3]福建农林大学食品科学学院,福州350002

出　　处：《分析试验室》2015年第9期1067-1071,共5页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科技项目(2014IK110);福建省科技攻关重点项目(2010Y6001);出入境检验检疫行业标准制(修)订计划项目(2013B128)资助

摘　　要：建立了超高效液相色谱-电喷雾串联质检测鸡组织中利巴韦林残留量的方法。采用10%乙腈-三氯乙酸溶液提取鸡组织中的利巴韦林,经磷酸酶水解,苯硼酸（PBA）固相萃取小柱净化,NUCLEOSHELL HILIC（3.0 mm×100 mm,2.7μm）色谱柱分离,采用电喷雾离子源串联质谱法,在正离子模式下以多反应监测（MRM）模式测定,同位素内标法定量。在优化条件下,利巴韦林在0.5～50 ng/m L范围内线性关系良好（r2〉0.99）,方法的检出限（信噪比为3）为0.1～0.3μg/kg,定量限（信噪比为10）为0.4～0.9μg/kg;鸡肉、鸡肝、鸡肾、鸡蛋和皮蛋在添加浓度1.0～10.0μg/kg范围内,其平均回收率为84.2%～92.6%,相对标准偏差（n=6）为5.0%～12%。An ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method has been established for the determination of ribavirin residues in chicken tissues. The sample was initially extracted in 10 % trichloroacetic acid （20 g/L）/acetonitrile solution, hydrolyzed by acid phosphatase, and then purified with the Bond Elut （PBA） SPE column. The chromatographic separation was achieved in gradient elution using a NUCLEOSHELL HILIC （3.0 mm × 100 mm, 2.7 μm） column with 5 mmol/L ammonium acetate （containing 0.2 % formic acid） and acetonitrile as mobile phase. A triple quadrupole with positive electrospray ionization was used for MS detection in MRM mode, and stable-isotope internal standard was adopted for quantitation. The calibration curve showed a good linearity ranging from 0.5 to 50 ng/mL, and the correlation coefficients （r2） were not lower than 0.99. The limit of detection （ LOQ, S/N = 3） and limit of quantification （LOQ, S/N = 10） of ribavirin were 0. 1 ～0.3 μg/kg and 0. 4 ～0.9 μg/kg, respectively. The average recovery varied from 84.2 % to 92.6 % at the spiked levels of 1.0 - 10.0 μg/kg in muscle, liver, kidney, egg and preserved egg. The relative standard deviations （RSDs） （n =6） were 5.0% ～ 12%.

关 键 词：高效液相色谱-电喷雾串联质谱法 利巴韦林 鸡组织 残留量 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]