快速液相色谱法及常规高效液相色谱法测定克林霉素磷酸酯及有关物.doc

快速液相色谱法及常规高效液相色谱法测定克林霉素磷酸酯及有关物 　 作者：张斗胜 李进 许明哲 王晨 姚蕾 相秉仁 胡昌勤 【摘要】 目的 比较分析快速液相色谱法(UFLC)与常规液相色谱法(HPLC)测定克林霉素磷酸酯含量及有关物质。 方法 UFLC法色谱柱采用Waters C18杂化柱(50mm×4.6mm，2.5μm)，流速1.5ml/min；HPLC法色谱柱采用Apollo C18(250mm×4.6mm，5μm)，流速1.0ml/min。两方法均以0.1mol/L磷酸二氢钾(85%的磷酸调pH3.5)∶乙腈∶甲醇(700∶150∶150)为流动相，检测波长210nm。结果 在UFLC法中，克林霉素磷酸酯在0.01～1.5mg/ml呈良好线性，r=0.9999；最低检测限为20ng；最低定量限为60ng；精密度RSD为0.41%。与HPLC法相比，该法测定克林霉素磷酸酯含量快速、准确、灵敏度高；但测定有关物质，其专属性、准确性不如HPLC法，杂质检出数目少且部分杂质分离不完全。结论 UFLC法可准确、快速、高效测定克林霉素磷酸酯含量，适合在工作量较大的检测项目如制剂含量、含量均匀度及溶出度中应用；但经简单方法转换建立的UFLC方法通常难以胜任对药物复杂体系如有关物质的分析。 【关键词】 快速液相色谱法； 高效液相色谱法； 克林霉素磷酸酯； 有关物质 ABSTRACT Objective To compare and analyze the UFLC and HPLC method for determination of the content of clindamycin phosphate and its related substances. Methods UFLC: a Waters C18 hybrid column was used, the flow rate was 1.5ml/min; HPLC: a Apollo C18 Column was applied, the flow rate was 1.0ml/min; 0.1mol/L potassium dihydrogen phosphate (pH was adjusted to 3.5 by 85% phosphoric acid)∶acetonitrile∶methanol (700∶150∶150, V/V) as mobile phase; the detective wavelength was 210nm. Results The linear range of clindamycin phosphate was 0.01 ～1.5 mg/ml, r=0.9999; the LOD was 20ng and the LOQ was 60ng, and RSD was 0.41%. The accuracy of UFLC method in determination the content of clindamycin phosphate was good, and it was more sensitive and rapid than HPLC, but in determination of related substances, it had a poor performance. Conclusion The UFLC method was proved to be simple, accurate, rapid and high efficient, so it could be applied to rapid analysis of the content of clindamycin phosphate in preparations that need detect the test items such as content, uniformity of dosage units, dissolution and so on, however this UFLC method was not suitable for determination of the related substances in the components. KEY WORDS Ultrafast liquid chromatography method; HPLC; Clindamycin phosphate; Related Substances 快速液相色谱(ultrafast liquid chromatography，UFLC)是一种新的快速分析技术，它与超高效液相色谱(ultraperformence liquid