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目的:采用反相高效液相色谱法对交沙霉素原料及交沙霉素片中的有关物质进行分析。方法:采用Ultimate-AQ-C18色谱柱(250 mm×4.6 mm,5μm),流动相A为0.2 mol·L-1四丁基硫酸氢铵-0.2 mol·L-1磷酸氢二钠(pH3.0)-乙腈-水(3∶5∶24∶68),流动相B为0.2 mol·L-1磷酸氢二钠一水合物(pH 3.0)-乙腈-水(5∶50∶45),线性梯度洗脱。流速为1.5 ml·min-1,检测波长为232 nm,柱温为50℃。结果:交沙霉素主峰与杂质A、B、C、D、E相邻各峰间分离度均较好;交沙霉素主峰与其保留时间为1.1倍处杂质峰的分离度大于1.7。交沙霉素最低检出限为1.43 ng。交沙霉素原料和交沙霉素片中杂质A、B含量在1.5%以下,杂质D所占比例在2.0%以下,杂质E所占比例在3.0%以下,交沙霉素其它最大杂质所占比例在1.0%以下,总杂质所占比例在12%以下。交沙霉素原料中杂质C所占比例在1.0%以下,而交沙霉素片中杂质C所占比例在3.0%以下。结论:本方法灵敏度高,重现性好,专属性强,结果准确可靠,可以有效地分析交沙霉素原料及交沙霉素片中有关物质。
OBJECTIVE: To analyze the related substances in jasamycin and jasminemycin tablets by reversed-phase high performance liquid chromatography. Methods: The column A-C18 (250 mm × 4.6 mm, 5 μm) was used as the mobile phase. The mobile phase A was 0.2 mol·L -1 tetrabutylammonium hydrogen sulfate-0.2 mol·L -1 disodium hydrogen phosphate (pH 3) 0) -acetonitrile-water (3: 5:24:68). The mobile phase B was 0.2 mol·L -1 disodium hydrogen phosphate monohydrate (pH 3.0) -acetonitrile-water Gradient elution. The flow rate was 1.5 ml · min-1, the detection wavelength was 232 nm and the column temperature was 50 ℃. Results: The main peak of jasminemycin was separated from the adjacent peaks of impurity A, B, C, D and E. The resolution of the peak of jasamycin was more than 1.7 when the main peak of jasminemycin and its retention time was 1.1 times. The detection limit of jasmomycin was 1.43 ng. Josamycin and jasamycin tablets jasamycin tablets impurity A, B content of 1.5% or less, the proportion of impurity D is less than 2.0%, the proportion of impurities E below 3.0%, jasamycin other maximum impurity The proportion of less than 1.0%, the total impurities accounted for less than 12%. The proportion of impurities C in josamycin raw material is less than 1.0%, while the proportion of impurity C in jasamycin is less than 3.0%. Conclusion: The method has high sensitivity, good reproducibility, strong specificity and accurate and reliable results, which can effectively analyze the related substances in josamycin and jasamycin tablets.