Roman Juliana, Breier Ana R, Steppe Martin
Post-Graduate Program of Pharmaceutical Sciences, Federal University of Rio Grande do Sul, Av. Ipiranga, 2752. Lab. 402, Porto Alegre-RS CEP, 90610-000, Brazil.
J Chromatogr Sci. 2011 Aug;49(7):540-6. doi: 10.1093/chrsci/49.7.540.
Reversed-phase high performance liquid chromatography (LC) method is developed for the assay of sodium montelukast in coated tables and its photodegradation kinetics. An isocratic LC separation is performed on a Zorbax XDB C18 column using a mobile phase of acetonitrile-methanol-water (pH 3.8) (75:10:15, v/v/v) at a flow rate of 0.8 mL/min and detection at 280 nm. The detector response for sodium montelukast is linear over the concentration range from 5-35 μg/mL (r = 0.9999). The specificity of the method is proved using stress conditions. The solutions are exposed to UV radiation (352 nm), alkaline and acid hydrolysis, oxidation, and temperature (80 °C). The intra- and inter-day precision show suitable results (RSD < 0.49%). The accuracy of analytical method is 100.04% (RSD = 0.44%). Detection and quantification limits are 0.10 and 0.32 μg/mL respectively. The robustness of the method is assured after small changes in chromatographic conditions. The kinetic of photodegradation using a LC method is established and it can be described by zero-order kinetics. This developed method show to be viable for the determination of sodium montelukast in pharmaceutical dosage form and satisfactory in the determination of the kinetics of degradation.
建立了反相高效液相色谱（LC）法用于测定包衣片中孟鲁司特钠及其光降解动力学。在Zorbax XDB C18柱上进行等度LC分离，流动相为乙腈 - 甲醇 - 水（pH 3.8）（75:10:15，v/v/v），流速为0.8 mL/min，检测波长为280 nm。孟鲁司特钠的检测器响应在5 - 35 μg/mL浓度范围内呈线性（r = 0.9999）。通过强制条件试验证明了该方法的专属性。溶液分别进行紫外辐射（352 nm）、酸碱水解、氧化和高温（80°C）处理。日内和日间精密度结果良好（RSD < 0.49%）。分析方法的准确度为100.04%（RSD = 0.44%）。检测限和定量限分别为0.10和0.32 μg/mL。在色谱条件稍有变化后，该方法的稳健性得到保证。建立了用LC法测定光降解动力学的方法，其光降解可用零级动力学描述。该方法对于药物剂型中孟鲁司特钠的测定是可行的，并且在降解动力学测定方面令人满意。
