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作 者:钱智磊[1] 周秋云[1] 陆磊[1] 张亮[1] 丁红梓[1] 王洁[1] 林霏申[2] 朱文玉[1]
机构地区:[1]南京市胸科医院药学部,南京210029 [2]南京市胸科医院八病区,南京210029
出 处:《西北药学杂志》2013年第6期611-614,共4页Northwest Pharmaceutical Journal
基 金:南京市科技发展指导性计划(药学项目)南京市药学会-常州四药医院药学科研基金(编号:2013YX015);南京市医学科技发展项目(编号:YKK11064);南京市胸科医院青年专业人才基金
摘 要:目的:建立快速、灵敏的同时测定人血浆中异烟肼、吡嗪酰胺和利福平的质量浓度的高效液相色谱法。方法血浆样品采用甲醇沉淀蛋白法萃取,采用C18色谱柱(150mm×4.6mm,5.0μm),用甲醇、乙腈、0.05mol·L-1KH2PO3水溶液(三乙胺调pH6.0)进行梯度洗脱,柱温40℃,进样量20μL,采用PDA紫外检测器。结果以峰面积外标法定量,异烟肼在0.20~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9998),吡嗪酰胺在0.20~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9999),利福平胶囊在0.40~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9996),回收率为85%~115%,日内、日间精密度RSD均<9.4%(n=5)。结论该方法专属性强、灵敏、准确,适用于同时测定人血浆样品中异烟肼、吡嗪酰胺和利福平的质量浓度。Objective To develop an HPLC method for the simultaneous determination of isoniazid ,rifampicin and pyrazinamide in human plasma .Methods The compounds and internal standard were extracted from the plasma by a protein precipitation procedure with methanol .The separation of the analytes was performed on a C18 column (150 mm × 4 .6 mm ,5 .0μm) at 40 ℃ ,using a gra-dient elution program with solvents consisting of methanol ,acetonitrile and 0.05 mol · L -1 KH2 PO3-H2O .The injection volume was 20 μL .The compounds were detected by PDA .Results Calibration curves in spiked plasma were linear at 0 .20-25 .6 ,0.20-25 .6 and 0 .40-25 .6 μg · mL - 1 for isoniazid ,rifampicin and pyrazinamide ,respectively .The recoveries were 85% ~115% ,and the intra-day and inter-day RSDs were 〈9 .4% .Conclusion The method is specific ,sensitive and accurate ,and it can be used for the simultaneous determination of isoniazid ,rifampicin and pyrazinamide in human plasma .
分 类 号:R945[医药卫生—微生物与生化药学]
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