RP-HPLC法测定甲磺酸帕珠沙星原料含量及其有关物质

Determination of the Content of Pazufloxacin Mesilate's Raw Materials and its Preparation by RP-HPLC

目的:反相高效液相色谱法测定甲磺酸帕珠沙星原料含量及其有关物质。方法:采用Hypersil C_(18)(5μm, 4.6m×250m)色谱柱,以0.1%磷酸(加0.0805g磷酸氢二钾):乙腈(85:15)为流动相,流速1.0mL·min^(-1),柱温30℃,于243nm波长处测定甲磺酸帕珠沙星含量及有关物质。40±2℃放置6个月、25±2℃放置12个月考察质量稳定性。结果:1.0-500μg·mL^(-1)内峰面积与浓度线性关系良好。样品溶液室温放置24h稳定,RSD<1.0%。甲磺酸帕珠沙星保留时间为7.012min,与有关物质分离度>1.5。三批原料含量平均值为99.8%,有关物质含量<1.0%。加速试验及长期放置质量稳定。结论:RP-HPLC法测定甲磺酸帕珠沙星原料含量及其有关物质简便,结果可靠,可用于甲磺酸帕珠沙星原料及其制剂的质量控制。

Objective:To determine the content of Pazufloxacin mesilate's raw materials and its preparation by RP -HPLC.Methods:A separation was performed on a Hypersil C_(18)(5μm,4.6mm×250mm)column,mobile phase are 0.1%phosphoric acid with 0.0805g di-potassium hydrogen phosphate and Acetonitrile(85:15),flow rate is 1.0mL·min^(-1),temperature of pillar is 30℃,detective wavelength is 243nm.Results:It is good linear in the concentration range of 5.000-1000μg·mL^(-1)of concentration and area.The sample solution is stable within 24h,the precision is good (RSD<1.0%),n=5.Retention time of sample solution is 7.012min,its resolution between related material is no more than 1.5.The average content of three batches of crude drug is 99.8%,and related material is no less than 1.0%.Accelerated test and long test prove crude drug is stable.Conclusions:It is simple and reliable to determine the content of Pazufloxacin mesilate's raw materials and its preparation by RP-HPLC.