HPLC法测定利福霉素钠注射液的有关物质

目的完善利福霉素钠注射液有关物质的测定方法。方法采用高效液相色谱法,选用waters C18色谱柱,流动相A：0.39%磷酸二氢钠溶液（用8.5%的氢氧化钠溶液调节pH值至7.5）-乙腈（90∶10）;流动相B：0.39%磷酸二氢钠溶液（用8.5%的氢氧化钠溶液调节pH值至7.5）-乙腈（30∶70）;梯度洗脱：0～40min流动相B的比例从20%增加到80%,保持5min后,于2min内流动相B的比例从80%减少至20%并保持8min;流速为1.0mL·min^-1,进样20μL,检测波长为254nm。结果经专属性试验、定量限、耐用性试验、溶液稳定性试验,认定方法可行。结论修订后的质量标准,其有效性及可控性与修订前比较,有了明显的提高,适用于利福霉素钠注射液有关物质的测定。

Determination of Related Substances of Rifamycin Sodium Injection by HPLC

Objective To perfect the method for determination of related substances of Rifamycin Sodium Injection. Methods A HPLC method with graduate elution was applied, equipped with Waters ODS C18 column, using acetonitrile-0.39% solution of sodium dehydrogenate phosphate （adjusted to pH 7.5 with dilute sodium hydroxide solution） （10：90） as mobile phase A and acetonitrile-0.39% solution of sodium dehydrogenate phosphate （adjusted to pH 7. 5 with dilute sodium hydroxide solution） （70 ： 30） as mobile phase B. Graduate elution： For 0;40 minutes, the proportion of mobile phase B increased linearly from 20% to 80%. After hold on for 5 minutes, within 2 minutes the proportion of mobile phase B decreased linearly from 80% to 20%. Then hold on for 8 minutes. Flow rate was 1.0mL·min^-1 and detective wavelength was 254nm. Results After specificity experiment, quantitative limits experiment, durability experiment and liquid stability experiment, the method is proved to be feasible. Conclusions The revised quality standard has obvious improvement in efficacy and controllability. It is practicable to apply the method for determination of related substances of Rifamycin Sodium Injection.