摘要
建立高效液相色谱法测定片剂中枸橼酸氯米芬及其异构体含量,并建立异构体定量核磁测定法。色谱柱为C_(18)柱(25 cm×4.6 mm,5μm),流动相为缓冲液(1%三乙胺溶液,用磷酸调节pH值至2.5)-甲醇(30∶70),流量为1.0 mL/min,检测波长为233 nm,进样体积为50μL,采用一维核磁共振氢谱对顺式异构体进行定量分析。枸橼酸氯米芬的质量浓度在0.02~0.10 mg/mL范围内与色谱峰面积线性关系良好。加标回收率为100.4%~100.9%,测定结果的相对标准偏差为0.18%(n=9)。在异构体含量计算中引入校正因子,可显著减小测定偏差。该方法适用于枸橼酸氯米芬片的质量评价。
A method was established for the determination of clomiphene citrate and cis-isomer content in clomiphene citrate tablet by HPLC,and a quantitative nuclear magnetic resonance(qNMR)method for the determination of cis-isomer content was set up C_(18) column(25 cm×4.6 mm,5μm)was used as chromatography column,buffer(1.0%Et3N solution,phosphoric acid was used to adjust pH at 2.5)-MeOH(30:70)was used as the mobile phase with the flow rate of 1.0 mL/min,the detection wavelength was 233 nm and the injection volume was 50μL.The cis-isomer content was confirmed by 1H NMR.The chromatograph peak area of clomiphene had excellent linear dependence relation in the range of 0.02-0.10 mg/mL.The standard addition recoveries were 100.4%-100.9%with the relative standard deviation of 0.18%(n=9).The relative correction factor was introduced in cis-isomer content calculation,which could reduce result bias significantly.This method is suitable for quality evaluation of clomiphene citrate tablet.
作者
邵鹏
刘双
王琳
张喆
SHAO Peng;LIU Shuang;WANG Lin;ZHANG Zhe(Beijing Institute for Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)
出处
《化学分析计量》
CAS
2024年第4期67-73,共7页
Chemical Analysis And Meterage
关键词
枸橼酸氯米芬
顺式异构体
高效液相色谱
定量核磁共振法
clomiphene citrate
cis-isomer
high performance liquid chromatography
quantitative nuclear magnetic resonance