HPLC法测定甲磺酸培氟沙星片含量及有关物质

Determination of Content and Related Substance in Pefloxacin Mesilate Tablets by HPLC

目的:建立高效液相色谱法测定甲磺酸培氟沙星片中药物及有关物质。方法:色谱柱为C18柱(150mm×6mm,5μm),流动相为乙腈-2.70g/L十六烷基三甲基溴化氨与6.18g/L硼酸溶液的混合溶液(用1mol/L氢氧化钠溶液准确调pH至8.30)-硫二甘醇(30∶70∶0.2),检测波长为273nm。结果:甲磺酸培氟沙星在17.18～85.90μg/mL范围内与峰面积呈良好的线性关系(r=0.9999),其平均回收率为99.50%、99.71%、99.62%,最低检测限和定量限分别为0.01989ng和0.08517ng,与杂质及喹诺酮类同系物能有效分离。结论:本方法操作简便、结果准确、专属性强,可用于甲磺酸培氟沙星片中药物含量及有关物质的检测。

Objective：To establish a method for the assay of pefloxacin mesilate tablets and its related substance by HPLC. Methods： The analysis was conducted by HPLC using a C18 （150 mm × 6 mm, 5 μm） column. The mobile phase was acetonitrile-mixture of 2.70 g/L cetyhrimethylammonium bromide with 6. 18 g/L boric acid solution （adjusted to pH 8. 30 with 1 mol/L sodium hydroxide）-2,2＇- thiodiglycol （30 ： 70 ： 0.2）. The detection wavelength was set at 273 nm. Results： The precision and stability were fine. The linear correlation of pefloxacin mesilate tablets was observed within the range of 17.18 - 85.90μg/mL （r = 0.9999）. The average recoveries were 99.50%, 99.71% and 99.62%. The limit of detection and quantification was 0. 01989 ng and 0. 08517 ng respectively. The resolution between the respective peaks of pefloxacin mesilate with the other peaks conformed to the requirements. Conclusions： The method is simple, accurate and specific, and reproducible for the assay of pefloxacin mesilate tablets and its related substance.