高效液相色谱-串联质谱法测定鸡肝中利巴韦林及其代谢物残留总量

Determination of total residues of ribavirin and its metabolites in chicken liver by HPLC-MS/MS

关键词:  鸡肝  利巴韦林  高效液相色谱-串联质谱

Key words:  chicken liver  ribavirin  HPLC-MS/MS

摘要:

建立了鸡肝组织中利巴韦林及其代谢物残留总量检测的高效液相色谱-串联质谱（HPLC-MS/MS）方法。鸡肝经磷酸酯酶水解、苯硼酸（PBA）固相萃取柱净化、C18色谱柱分离、电喷雾离子化（ESI+）和选择反应监测（SRM）方式采集，并以13C5-利巴韦林为同位素内标定量。该方法的检出限为0.5 ng/g；利巴韦林的测定在0.5 ng/mL～20 ng/mL 范围内线性关系良好，线性相关指数r为0.9997；在1.0 ng/g、2.0 ng/g和10 ng/g三个添加浓度的平均回收率为66.8%～110.3%，批内相对标准偏差6.8%～11.7%，批间相对标准偏差7.3%～10.1%。

Abstract:

A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) method has been established for the determination of the total residues of ribavirin and its metabolites in chicken liver. The samples of chicken liver were digested by acid phosphatase, cleaned through phenyl boronic acid(PBA) cartridges and separated through a C18 column. Mass spectrometry condition: electrospray ionization(ESI+) and selected reaction monitoring (SRM) mode. The detection used 13C5- ribavirin as the isotopic internal standard. The limit of detection(LOD) of the method was 0.5 ng/g. The calibration curve has good linear within the range of ribavirin concentration from 0.5 ng/mL to 20 ng/mL, and the correlation coefficient r was 0.9997. The average recoveries from spiked chicken liver at three concentrations 1.0 ng/g, 2.0ng/g and 10 ng/g ranged from 66.8% to 110.3%, and the within- and between-run relative standard deviations(RSDs) were 6.8～11.7% and 7.3～10.1%, respectively.