摘要
Abstract
To effectively detect the five main impurity components—Desloratadine Pyridine N-Oxide,Desloratadine Impurity Ⅰ,Formyl Desloratadine,Iso Desloratadine,and Loratadine—in Desloratadine oral solution,a reliable and efficient high-performance liquid chromatography(HPLC)method was developed and fully validated.Due to significant differences in polarity and hydrophobicity among these impurities,the gradient elution procedure was systematically optimized to achieve complete baseline separation and accurate simultaneous quantification without interference from the main drug component or formulation excipients.Chromatographic separation was performed on a GL Sciences C18 column(250 mm×4.6 mm,5 μm).Mobile phase was A consisted of 0.25%(mass fraction)sodium dodecyl sulfate aqueous solution,and mobile phase B was acetonitrile.The optimized gradient elution program was as follows:0～20 min,60%A;20～25 min,60%～50%A;25～50 min,60%A;50～51 min,60%～50%A;51～60 min,50%A.The flow rate was maintained at 1.0 mL/min,the column temperature was set at 35℃,the detection wavelength was 280 nm,and the injection volume was 100 μL.Under these conditions,all five impurities exhibited sharp,symmetrical peaks with resolution values greater than 1.5 between adjacent peaks.The mass concentrations of the five main impurities showed good linear relationships with the corresponding peak areas within their respective ranges,with correlation coefficients all above 0.999.The limits of quantification ranged from 0.01 to 0.02 μg/mL,demonstrating high sensitivity suitable for trace impurity analysis in complex pharmaceutical matrices.Accuracy was evaluated through spike recovery experiments at three concentration levels(low,medium,and high).The average recoveries ranged from 94.7%to 103.3%,indicating good accuracy.Precision was confirmed by relative standard deviations of less than 3.0%(n=9),demonstrating excellent repeatability and intermediate precision.System suitability parameters,including theoretical plate numbers,tailing factors,and retention time stability,were all within acceptable limits.In conclusion,the established HPLC method is efficient,stable,accurate,and robust.It enables the simultaneous quantitative determination of the five major impurity components in Desloratadine oral solution.This method provides reliable and practical technical support for routine quality control,long-term stability studies,and regulatory compliance assessment of Desloratadine oral solution in pharmaceutical manufacturing and quality assurance environments.关键词
高效液相色谱法/梯度洗脱/地氯雷他定口服溶液/杂质检测/质量控制Key words
HPLC/gradient elution/Desloratadine oral solution/impurity testing/quality control分类
化学化工
