HPLC法测定3个厂家生产的硫酸氢氯吡格雷片中有效成分及有关物质

HPLC in determination of effective contents and related substances in clopidogrel hydrogen sulfate produced by 3 manufacturers

目的建立高效液相色谱法测定硫酸氢氯吡格雷片中有效成分S型氯吡格雷及有关物质R型氯吡格雷含量的方法，并比较3个厂家生产的氯吡格雷片中2种成分含量的差异。方法色谱条件：ULTRONES-OVM手性色谱柱（4．6mm×150mm，5μm），乙腈-0．01mol／L磷酸二氢钾溶液（20：80）为流动相，流速为1mL／min，柱温17℃，检测波长220nm。结果硫酸氢氯吡格雷S型及R型分别在50～117mg／L和1．52～30．4mg／L范围内线性关系良好（相关系数r均为0．9998），精密度良好，平均回收率分别为99．7％和98．8％，供试品溶液室温放置12h稳定；3个厂家生产的硫酸氢氯吡格雷片S型及R型的含量均符合药典要求。结论本方法准确度好，专属性强，可用于硫酸氢氯吡格雷片的质量控制。

Objective To establish a high performance liquid chromatography （HPLC） method for quantitative determination of S-clopidogrel and its related substance R-clopidogrel in clopidogrel tablets, and to compare their contents between clopidogrel tablets produced by three different manufacturers. Methods An ULTRON ES-OVM column （ 4.6 mm × 150 mm,5 μm） was used in this study. The mobile phase consisted of a mixture of acetonitrile and 0. 01 mol/L potassium dihydrogen phosphate solution （20 ： 80）. The flow-rate was 1 mL/min, with the column temperature being 17℃ and the UV detection wave lenth being 220 nm. Results S-clopidogrel and its related substance R-clopidogrel were in good linear relationship within 50-117 mg/L and 1. 52-30. 04 mg/L, respectively （both r= 0. 999 8）. The precision of our method was satisfactory and the average recoveries were 99. 7% and 98. 8%, respectively. The test solution remained stable for 12 h. S-clopidogrel and R-clopidogrel in clopidogrel tablets produced by three manufacturers were in line with the quality requirements of pharmacopoeia. Conclusion Our method is accurate and has good specificity. It can be used for the quality control of clopidogrel tablets.