HPLC测定交沙霉素中的有关物质

Determination of the related substance of Josamycin by HPLC

目的采用梯度洗脱HPLC法测定不同厂家交沙霉素中的有关物质。方法采用Waters XBridgeTMC18色谱柱(250 mm×4.6 mm,5μm),流动相A为67.9 g·L-1四丁基硫酸氢铵-27.6 g·L-1磷酸氢二钠水合物(pH3)-乙腈-水(3∶5∶24∶68)、流动相B为27.6 g·L-1磷酸氢二钠一水合物(pH3)-乙腈-水(5∶50∶45),线性梯度洗脱,检测波长232 nm,柱温50℃。结果交沙霉素主峰及杂质A～E与各相邻峰间的分离度均较好,交沙霉素的最低检出限为1.43 ng。结论与《中国药典》2010年版收载的方法比较,所用方法针对特定杂质进行控制,方法简便可靠、专属性好,适用于控制交沙霉素中的有关物质。

OBJECTIVE To establish a gradient HPLC method for the related substance of Josamycin from different manufacturers. METHODS The column was Waters XBridgeTM C 18 （250 mm× 4.6 mm,5 μm）with mobile phase A ：67.9 g·L^- 1 tetrabutylammoni- um hydrogen sulphate - 27.6 g· L^- 1 sodium hydrogen phosphate monohydrate （ pH3 ） - acetonitrile - water （ 3 ： 5 ： 24 ： 68 ）, and mobile phase B ： 27.6 g·L ^- 1 sodium hydrogen phosphate monohydrate （ pH3 ） - aeetonitrile - water （ 5 ： 50 ： 45 ） with linear gradient elution. The detection wavelength was 232 rim. The column temperature was 50 ℃. RESULTS Good resolution for Josamycin and related substances was obtained. The detection limit of Josamycin was 1.43 ng. CONCLUSION Compared with ChP 2010, the method in this paper is simple and reliable for the control of specific impurities and suitable for the determination of related substances of Josamycin.