加校正因子的主成分自身对照法测定青霉素V钾片有关物质及.doc

PAGE  加校正因子的主成分自身对照法测定青霉素V钾片有关物质及稳定性的考察注：与文章主题关联性不大,经与作者沟通，作者对文章作了相应修改。 刘琳1，李慧1，张菁2，刘云1*，刘珠1（1.石家庄市食品药品检验中心，石家庄 050031；2.河北省药品检验研究院，石家庄 050011） 摘要 目的：建立加校正因子的主成分自身对照法测定青霉素V钾片有关物质的含量，并考察其稳定性。方法：采用XBridge Shield RP-18C18色谱柱（250mm×4.6mm×250mm，5μm），以磷酸盐缓冲液（pH3.5）-甲醇-水为流动相，梯度洗脱；检测波长268nm；测定特定杂质4-羟基苯氧甲基青青霉素V应为4-羟基苯氧甲基青霉素V吧？核实- 相对于青霉素V的校正因子，并进行定量分析，同时对样品的稳定性进行考察。结果：4-羟基苯氧甲基青霉素4-羟基氧甲基青青霉素V杂质的相对保留时间为0.42，校正因子为1.41；加校正因子的主成分自身对照法与外标法测定的结果无显著性差异。稳定性考察显示在超出药品规定的贮存条件下，有关物质含量、水分值逐渐增大。结论：该方法简便快速，可准确测定青霉素V钾片中特定杂质的含量。；贮存条件对其内在质量存在影响，建议在生产和贮存过程中控制贮存条件，以控制制剂的质量。 关键词：校正因子HPLC法；青霉素V钾片；4-羟基苯氧甲基青霉素4-羟基青霉素V；有关物质 The Method of Main Component Self-Control Corrected with Calibration Factor Was UsedMain Component self-Compare with Calibration Factor Method for Determination of Related Substances and Stability Test in Phenoxymethylpenicillin Potassium Tablets Liu Lin1, Li Hui1, Zhang Jing2, Liu Yun1*, Liu zhu1（1.Shijiazhuang Institute for Food and Drug Control, Shijiazhuang 050031; 2.Hebei Provincial Institute for Drug Control, Shijiazhuang 050011） Abstract Objective: To establish the method of main component self-controlcompare corrected with calibration factor method to determine the contents of related substances in Phenoxymethylpenicillin Potassium Tablets, and investigate its stability. Methods: The assay was performed on a Chromatographic condition: XBridge Shield RP-18C18 column (250mm×4.6mm×250mm, ，5μm), with phosphate buffer solution (pH 3.5)-methanol-water as mobile phase with, gradient elution,. Tthe detection wavelength as was at 268nm. Determine Tthe correction factor of 4-Hydroxyphenoxymethylpenicillin relative to Phenoxymethylpenicillin, then make the quantitative analysis of the impurity.was determined between impurity 4-Hydroxyphenoxymethylpenicillin and Phenoxymethylpenicillin, and Tto determine its content and investigate its stability. . Results: The relative retention time and the correction factor of between the impurity of 4-Hydroxyphenoxymethylpenicillin wereas