HPLC法测定富马酸贝达喹啉片的含量及有关物质  

Determination of the Content of Bedaquiline Fumarate Tablets and Its Related Substances by HPLC

作　　者：陈韡彬 江宁宇[1] 魏宗有[1] 王娟[1] 陈宇翔[1] CHEN Wei-bin;JIANG Ning-yu;WEI Zong-you;WANG Juan;CHEN Yu-xiang(Fujian Institute of Microbiology,Fuzhou 350007,China)

机构地区：[1]福建省微生物研究所,福建福州350007

出　　处：《海峡药学》2022年第2期78-81,共4页Strait Pharmaceutical Journal

摘　　要：目的建立HPLC法测定富马酸贝达喹啉片的含量及有关物质,为其质量控制提供依据。方法以10 mmol·L^(-1)乙酸铵溶液-20%乙酸水溶液(200∶1)为溶液A,乙腈-乙醇-20%乙酸水溶液(600∶400∶2.5)为溶液B,检测波长为230 nm,有关物质采用Gemini C_(18)色谱柱(250×4.6 mm,5μm),流动相为溶液A-溶液B(45∶55),流速1.0 mL·min^(-1),柱温60℃。含量采用YMC-Pack Pro C_(18)色谱柱(150×3.0 mm,5μm),流动相为溶液A-溶液B(40∶60),流速0.5 mL·min^(-1),柱温35℃。结果有关物质方法富马酸贝达喹啉与相邻杂质以及各杂质峰间的分离均良好;检测限为0.26 ng,定量限为0.90 ng;含量方法富马酸贝达喹啉质量浓度在20.1~140.6μg·mL^(-1)范围内线性关系良好(r=1.0000);中间精密度RSD为0.94%;平均回收率为100.9%,RSD为0.25%。结论所建HPLC方法能准确地进行定性、定量分析,可用于富马酸贝达喹啉片的质量控制。OBJECTIVE HPLC method was established for the determination of the content of bedaquiline fumarate tablets and its related substances to provide basis for quality control.METHODS The 10 mmol·L^(-1) ammonium acetate solution-20%acetic acid solution(200∶1)was used as solution A,and the acetonitrile-ethanol-20%acetic acid solution(600∶400∶2.5)was used as solution B.The detection wavelength was 230 nm.A Gemini C_(18)(250×4.6 mm,5μm)column was adopted for the related substances.The mobile phase was solution A-solution B(45∶55).The flow rate was 1.0 mL·min^(-1) and column temperature was 60℃.A YMC-Pack Pro C_(18) column(150×3.0 mm,5μm)was adopted for content determination.The mobile phase was solution A-solution B(40∶60).The flow rate was 0.5 mL·min^(-1) and column temperature was 35℃.RESULTS Bedaquiline fumarate and all impurities were well separated by related substance method.The LOD was 0.26 ng and the LOQ was 0.90 ng.The linearity of bedaquiline fumarate was fine in the range of 20.1-140.6μg·mL^(-1) with the correlation coefficient of 1.0000.The RSD of intermediate precision was 0.94%.The average recovery was 100.9%and RSD was 0.25%.CONCLUSION The new established HPLC methods can accurately carry out qualitative and quantitative analysis.It can be used for quality control of bedaquiline fumarate tablets.

关 键 词：富马酸贝达喹啉 片剂 含量测定 有关物质 高效液相色谱 

分 类 号：R927[医药卫生—药学]