Li Junmei, Jiang Ye, Sun Ting, Ren Shumeng
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang City, PR China.
J Pharm Biomed Anal. 2008 Aug 5;47(4-5):929-33. doi: 10.1016/j.jpba.2008.02.023. Epub 2008 Feb 29.
A rapid, simple and specific method has been developed and validated for the assay of ciclopirox olamine in pharmaceutical formulations using micellar electrokinetic capillary chromatography (MEKC). The key factors, including pH, buffer concentration and buffer additive, sodium dodecyl sulfate (SDS) concentration, applied voltage and injection time have been systematically investigated in a fused silica capillary (i.d. 50 microm, total length 45 cm and effective length 38 cm) with UV detection at 298 nm. Optimized conditions have been established on the basis of the experimental results. The buffer contains 200 mM borate, 20 mM SDS and 2 mg mL(-1) EDTA at pH 8.0 and the applied voltage is 20 kV with hydrodynamics sample injection (15 cm high for 5s). The method has been validated with respect to its specificity, linearity, limits of detection, and quantification, precision and accuracy. The total analysis time was less than 10 min with good peak shape for ciclopirox olamine, which eluted at 3.6 min. Degradation of the ciclopirox olamine was forced using different conditions. These were using hydrogen peroxide, acidic and basic conditions, heat and light. The degradation products so produced showed no interference with ciclopirox olamine. A linear standard curve was established over the concentration range 31.3-2.00 x 10(3) microg mL(-1) of ciclopirox olamine in running buffer with a correlation coefficient (r) of 0.9999. The limits of quantification and detection were 31.3 and 9.36 microg mL(-1), respectively. The proposed method has been successfully used for the quantitative determination of ciclopirox olamine in pharmaceutical suppository and cream formulations.
已开发并验证了一种快速、简单且特异的方法，用于采用胶束电动毛细管色谱法（MEKC）测定药物制剂中的环吡酮胺。在一根内径50微米、总长度45厘米且有效长度38厘米的熔融石英毛细管中，于298纳米处进行紫外检测，系统研究了包括pH、缓冲液浓度和缓冲添加剂、十二烷基硫酸钠（SDS）浓度、施加电压和进样时间等关键因素。根据实验结果建立了优化条件。缓冲液包含200 mM硼酸盐、20 mM SDS和2 mg mL⁻¹ EDTA，pH为8.0，施加电压为20 kV，采用流体动力学进样（15厘米高，进样5秒）。该方法在特异性、线性、检测限和定量限、精密度和准确度方面均已得到验证。环吡酮胺的总分析时间不到10分钟，峰形良好，在3.6分钟时洗脱。采用不同条件强制使环吡酮胺降解，这些条件包括使用过氧化氢、酸性和碱性条件、加热和光照。如此产生的降解产物对环吡酮胺无干扰。在运行缓冲液中环吡酮胺浓度范围为31.3 - 2.00×10³ μg mL⁻¹时建立了线性标准曲线，相关系数（r）为0.9999。定量限和检测限分别为31.3和9.36 μg mL⁻¹。所提出的方法已成功用于药物栓剂和乳膏制剂中环吡酮胺的定量测定。
