RP-HPLC测定双氯西林钠的含量

Determination of dicloxacillin sodium in the presence of its degradants by RP-HPLC

目的 建立一种适用于双氯西林钠含量测定方法。方法 采用RP -HPLC法 ,ShimadzuODS柱 (2 5 0mm× 4 .6mm ,10μm) ,甲醇 - 0 .0 2mol·L-1磷酸二氢钾溶液 (5 5∶4 5 ,加入 0 .0 1mol·L-1的四甲基氯化铵 ,调节pH 5 .0 )为流动相 ,检测波长为 2 2 5nm ,柱温 35℃。采用导数色谱法鉴定了色谱峰纯度 ,并与美国药典收载的色谱条件进行了比较。结果 双氯西林钠在 30～6 0 0 μg·ml-1范围内 ,峰面积与浓度的线性关系良好 (r =0 .9998) ;平均回收率为 10 0 .37% ,重复性试验RSD =0 .37% (n =6 )。与美国药典收载的色谱条件相比较 ,双氯西林钠与相邻杂质分离更完全。结论 所建立的方法简便、准确、重复性好 ,可作为双氯西林钠稳定性及降解动力学研究的含量测定方法。

OBJECTIVE To establish an HPLC method applicable to the analysis of dicloxacillin sodium in the presence of its degradants.METHODS Peak homogeneity of the resolving drug peak was assessed by the shape of the derivative spectroscopy.Shimadzu ODS column(200 mm×4.6mm,5μm) was used.The mobile phase was methanol-0.02 mol·L -1 monobasic potassium phosphate (55∶45,added 0.01 mol·L -1 tetramethylammonium chloride,adjust to pH 5.0) and the flow rate was 1.0 ml·min -1.The UV detective wavelength was 225 nm.RESULTS The calibration curve was linear in the range of 30-600 μg·ml -1 (r=0.9998).The average recovery was 100.37% with RSD of 0.52%.The method precision was 0.37%(n=6).CONCLUSION The method is selective,simple and accurate.It is applicable to the analysis of dicloxacillin sodium in the presence of its degradants.