RP-HPLC法测定环吡酮涂剂的含量及有关物质

Determination of ciclopirox and its related substances by RP-HPLC

目的 用反相高效液相色谱法测定环吡酮涂剂的含量及有关物质。方法 采用 Purospher C1 8柱 ,以流动相 A(乙腈 ) -流动相 B(含 0 .0 2 5 mol/ L 柠檬酸、0 .0 0 2 5 mol/ L 乙二胺四乙酸二钠 ,Na OH调p H6 .5 ) (35∶ 6 5 )的混合液作为流动相 ,流速为 1.0 ml/ min,检测波长 30 3nm,柱温 30℃。结果 环吡酮在 10 0～ 30 0 μg/ ml范围内 ,浓度与峰面积的线性关系良好 (r=0 .9999) ,环吡酮的平均回收率为 10 0 .5 % ,RSD为0 .5 8% (n=9)。最低检测限 ,吡啶酮为 0 .1ng,吡喃酮为 0 .3ng。结论 本方法简便 ,快速 ,结果准确 ,可靠 ,重现性好 ,可供本品质量控制用。

Objetive To establish a RP-HPLC method for the determination of ciclopirox and its related substances. Methods The separation was performed on a Purospher C 18 column (5μm, 4.0mm×125mm) with acetonitrile and a solution of 0.025mol/L citric acid monohydrate and disodium ethylenediamine tetracetate in 1000ml pure water (adjust to pH6.5 with 10% NaOH) (35∶65) as the mobile phase. The flow rate was 1.0ml/min, the detection wavelength was set at 303nm and the column temperature maintained at 30℃. Result The calibration curve was linear in the concentration range of 100～300μg/ml, r=0.9999. The average recovery rate was 100.5% and RSD 0.58% (n=9). The detection limits were 0.1ng for pyridone and 0.3ng for pyrone respectively. Conclusions The method is simple, rapid, and good reproducibility. It may be used for quality control of the drug.