山西医科大学学报2024，Vol.55Issue(9)：1207-1213,7.DOI:10.13753/j.issn.1007-6611.2024.09.015
HPLC法测定氯法齐明原料药中有关物质的含量
Determination of relevant substances in Clofazimine active pharmaceutical ingredients by HPLC method
摘要
Abstract
Objective To establish a method for determining the contents of substances in Clofazimine active pharmaceutical ingredient(API).Methods High performance liquid chromatography(HPLC)was performed on a Caprisil C8-P(250 mm×4.6 mm,5 μm)column.And 4.5 g of sodium dodecyl sulfate,1.7 g of tetrabutylammonium hydrogensulfate and 1.77 g of disodium hydrogen phosphate dodecahydrate were dissolved in 1 000 mL of water,then adjusted to pH=3.0 with dilute phosphoric acid,and then the above solution was mixed with acetonitrile in the ratio of 35∶65 as the mobile phase.The flow rate was 1.0 mL/min,the detection wavelength was 280 nm,the column temperature was 30℃,and the injection volume was 20 μL.Methodological validation of this HPLC method was carried out.The contents of relevant substances in three batches of Chlorpheniramine API were determined,and the results measured by the external standard method were compared with the principal component self-control method with correction factor.Results There was a good linear relationship for Clofazimine,impurity A and impurity B in the range of 0.019-0.959 μg/mL,0.017-0.858 μg/mL,and 0.060-2.995 μg/mL,respectively(all R2＞0.999),the limits of detection were 0.22 ng,0.27 ng,and 0.23 ng,and the limits of quantification were 0.72 ng,0.91 ng,and 0.76 ng,respectively.The RSDs of precision,repeatability,stability and durability experi-ments were all less than 5%,and the average recoveries were 93.37%-98.17%.Impurity A and impurity B were detected in all three batches of Clofazimine raw material,with the content range of 0.013%-0.014%for impurity A,and 0.025%-0.026%for impurity B.There was no significant difference in the contents of related substances determined by the principal components self-control method with correction factor and the external standard method.Conclusion The established HPLC method is convenient,efficient and accurate,and can be used for determining the contents of the relevant substances in Clofazimine API.The principal component self-control method with correction factor is low cost and practical.关键词
高效液相色谱法/氯法齐明原料药/有关物质/含量测定/方法学验证/加校正因子的主成分自身对照法Key words
high-performance liquid chromatography/Clofazimine API/related substances/content determination/methodo-logy validation/principal component self-control with correction factor分类
药学引用本文复制引用
王文涛,高彦红,张升盛,王二兵,赵正保,曲婷丽..HPLC法测定氯法齐明原料药中有关物质的含量[J].山西医科大学学报,2024,55(9):1207-1213,7.基金项目
山西省重点研发项目(202102130501023) （202102130501023）
太原市科技局"双百攻关行动"首批关键核心技术攻关"揭榜挂帅"项目(2024TYJB0147) （2024TYJB0147）
山西省技术创新中心项目(202104010911006) （202104010911006）
山西省科技厅基础研究项目(20210302124586) （20210302124586）
