摘要
目的探讨在ODS柱上分离测定枸橼酸氯米芬的反相高效液相色谱法。方法采用色谱柱A[Phenonex H yperClone ODS 120A(150m m×4.6m m,5μm)]和色谱柱B D[ionex Krom asilODS1(250m m×4.6m m,5μm)],以不同比例的甲醇或乙腈与不同pH值缓冲液的混合溶液为流动相,试验多种色谱条件下的色谱行为。结果当采用色谱柱B,流动相为0.035m olL/磷酸三乙胺缓冲液(pH=6.2)-甲醇(15∶85),流速为1.50m L m/in,检测波长为290nm时,枸橼酸氯米芬顺反式异构体的保留时间分别为14.7m in和16.1m in,理论塔板数分别为4810和4571,拖尾因子分别为1.25和1.17,分离度为1.6,与10种有关物质达到良好的基线分离。结论方法简便、快速,适用于枸橼酸氯米芬及其制剂的质量控制。
Objective To develop a RP- HPLC method for the isolation and determination of clomiphene citrate on ODS Columns and its related substances. Methods Column A [Phenonex Hyper Clone ODS 120A （150 mm × 4. 6 mm, 5 μm）] and column B [Dionex Kromasil ODS1（250 mm ×4.6 ram,5μm）]. The mobile phases were different mixtures of methanol or acetonitrile and buffer solutions of pH 2. 5, 4.1 or 6. 2. Clomiphene citrate was tested with several chromatographic conditions. Results The chromatographic procedure was carried out on column B, the mobile phase was methanol-0. 035 mol/L phosphoric acid previously adjusted to pH=6.2 with triethylamine （85：15） with flow rate of 1.50 mL/min. The detection wavelength was 290 nm. For the （E）-and （Z） - geometric isomers of clomiphene citrate, the retention times were 14.7 min and 16. 1 rain, the theoretical plates were 4 810 and 4 571, the tailing factors were 1.25 and 1.17. The resolution between （E） isomer and （Z） isomer was 1.6. Ten related substances were isolated on baseline. Conclusion The method is simple, rapid and can be used for the isolation and determination of clomiphene citrate and its related substances.
出处
《中国药业》
CAS
2006年第14期22-23,共2页
China Pharmaceuticals
