摘要
目的:建立流感疫苗中去氧胆酸残留量的LC-MS/MS测定方法。方法:采用液相色谱-电喷雾串联四极杆质谱仪,多离子反应监测(MRM)定量法。用胆酸作内标,通过对试样净化预处理、色谱条件、质谱参数等的优化选择和方法回收率、精密度等的验证,建立了定量测定流感疫苗中去氧胆酸残留的理想方法。结果:方法检出限为0.005mg·L^(-1),定量限为0.010mg·L^(-1),在0.005～1.00mg·L^(-1)线性范围内,相关系数r为0.9998,回收率大于98.0%,方法精密度RSD小于4.0%(n=6)。结论:采用液相色谱-电喷雾串联四极杆质谱仪,可快速测定流感疫苗中的去氧胆酸,结果准确可靠,重复性好,灵敏度高,建立的方法可以准确测定流感疫苗中去氧胆酸的残留量。
Objective：To establish a method for the detection of deoxycholate residues in split influenza virus vaccine. Method： The analytes were separated and detected by liquid chromatography - electrospray ionization tandem mass spectrometry（ LC- ESI- MS/MS）,mass spectral acquisition was done in the negative ion mode by Multiple reaction monitoring （MRM）. The sample was processed by cleaned - up and concentrated by SPE on a HLB column, the chromatography was performed by reversed -phase HPLC on a C,s column with MRM detection, the mobile phase was methanol- water （80： 20）. Result：The LOD was 0. 005 mg·L^-1, LOQ was 0. 010 mg·L^-1, linear range was 0. 005 - 1.00 mg ·L^-1 ,r =0. 9998 ,the average recovery was above 98.0% ,RSD 〈4.0% （n =6）. Conclusion：The method is efficient in detecting deoxycholate residues in split influenza virus vaccine, with high sensitivity, good reproducibility and selectivity, simple operation.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第4期548-551,共4页
Chinese Journal of Pharmaceutical Analysis
