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HPLC-ESI/MS法测定人血浆中枸橼酸喷托维林的方法学研究

HPLC-ESI/MS determination of pentoxyverine citrate in human plasma
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摘要 目的:建立HPLC-ESI/MS分析方法测定人血浆中枸橼酸喷托维林的浓度。方法:采用Inertsil ODS-3C18(150mm×2.1mm,5μm)色谱柱,流动相为0.1mol.L-1醋酸铵溶液(甲酸调pH4.4)-甲醇(35:65),流速0.20mL.min-1,柱温为25℃;内标为盐酸洛拉曲克;质谱用电喷雾电离源正离子模式(ESI+),选择离子监测(SIR);样品用固相萃取法处理。结果:枸橼酸喷托维林的线性范围为0.78~300ng.mL-1,r=0.998,喷托维林提取回收率>70%,相对回收率在85%~115%范围内,日内、日间RSD均<15%。结论:该方法专属性强,灵敏度高,结果准确,可用于枸橼酸喷托维林血药浓度测定。 Objective:To establish an HPLC-ESI/MS method for the determination of pentoxyverine citrate in human plasma.Methods:The separation of the analytes was performed on Inertsil ODS-3 C18(150 mm×2.1 mm,5 μm) column using a mobile phase consisting of 0.1 mol·L-1 ammonium acetate solution(pH 4.4,adjusted by formic acid) and methanol (35:65) with a flow rate of 0.20 mL·min-1 at column temperature of 25 ℃.Nolatrexed dihydrochloride was used as internal standard.The compounds were detected in the selected ion recording(SIR)with electrospray ionization source in positive ion(ESI+).The samples were extracted using solid phase extraction column.Results:The linear range of pentoxyverine citrate was 0.78-300 ng·mL-1 with r=0.998.The extracted recovery rate of pentoxyverine was larger than 70%,and the relative recovery rates were 85%-115%;The intra-and inter-day RSDs were less than 15%.Conclusion:This method is specific,sensitive and accurate for the determination of pentoxyverine citrate concentration in human plasma.
出处 《药物分析杂志》 CAS CSCD 北大核心 2010年第5期853-857,共5页 Chinese Journal of Pharmaceutical Analysis
基金 教育部新世纪优秀人才计划项目(NCET-06-0753) 霍英东高等院校青年教师基金项目(111045)
关键词 枸橼酸喷托维林 HPLC-ESI/MS 固相萃取 pentoxyverine citrate HPLC-ESI/MS solid phase extraction
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