克拉霉素干混悬剂有关物质方法研究

目的 建立RP-HPLC法，测定克拉霉素干混悬剂的有关物质。方法 采用Agilent 1260 Infinity LC液相色谱仪，色谱柱为YMC C18(250mm×4.6mm, 5μm)柱，以0.033mol/L磷酸二氢钾溶液-乙腈(55:45)(用85%磷酸溶液或2mol/L氢氧化钾溶液调节pH值至5.4)为流动相，检测波长205nm，柱温50℃。结果 克拉霉素与9个已知杂质及其他未知杂质均能达到有效分离，克拉霉素及杂质E的线性范围分别为2~1000μg/mL(r=1.000)、0.9~6.75μg/mL(r=0.998)；供试品溶液在室温25℃下的12h基本稳定。结论 本方法灵敏，准确，专属性强，重现性好，可用于克拉霉素干混悬剂有关物质的测定。

Study on the related substances in clarithromycin for dry oral suspension

Objective To develop an RP-HPLC method for the determination of related substances in clarithromycin for oral suspension. Methods The chromatographic separation was achieved on a YMC C18 (250mm×4.6mm, 5μm) with the Agilent 1260 liquid chromatography system. The mobile phases consisted of 0.033mol/L potassium dihydrogen phosphate solution-acetonitrile (55:45) (pH value is adjusted to 5.4). The detection wavelength was 205nm, and the column temperature was 50℃. Results Good separation between clarithromycin and nine identified impurities and other unknown impurities could be achieved. Good linear relationship was observed in the concentration range of 2~1000μg/mL (r=1.000) for clarithromycin, 0.9~6.75μg/mL (r=0.998) for 6,11-di-O-methyl-erythromycin A(impurity E). Sample solutions were stable at 25℃ within 12 hours. Conclusion The method is sensitive, accurate, specific and reproducible, which can serve as a reliable analytical method for the determination of related substances in clarithromycin for oral