复方感冒灵颗粒多指标成分测定方法的建立及综合质量评价

Multiple content determination of compoumd Ganmaoling granules and comprehensive quality evaluation

目的建立HPLC法测定复方感冒灵颗粒中对乙酰氨基酚、咖啡因、马来酸氯苯那敏、蒙花苷的含量。方法对乙酰氨基酚采用Welchrom C_(18)色谱柱(250 mm×4.6 mm,5 μm);流动相水(含0.5%磷酸和0.4%三乙胺溶液)-乙腈(94∶6);流速1.0 mL·min^(-1);检测波长244 nm;柱温30℃。咖啡因和马来酸氯苯那敏采用Sepax Amethyst C_(18)-H色谱柱(250 mm×4.6mm,5 μm);流动相水(含0.5%磷酸和0.4%三乙胺溶液)-乙腈(93∶7);流速1.0 mL·min^(-1);检测波长264 nm;柱温30℃。蒙花苷采用Welchrom C_(18)色谱柱(250 mm×4.6 mm,5 μm);流动相甲醇-水-冰醋酸(26∶23∶1);流速1.0 mL·min^(-1);检测波长334 nm;柱温30℃。结果 4种成分在各自对应的线性浓度范围内与峰面积线性关系良好(r均≥0.9991);平均回收率在97.08%~104.37%,RSD在0.50%~3.8%。10批复方感冒灵颗粒的综合评价函数f值在-5.76~-5.26,RSD为3.7%。结论该方法准确、重复性良好,可用于复方感冒灵颗粒中4种成分含量的测定,综合质量评价表明10批次复方感冒灵颗粒质量稳定可控。

Objective To establish an HPLC method to determine the content of paracetamol,caffeine,chlorpheniramine maleate and linarin in compound Ganmaoling granules.Methods Welchrom C_(18) column(250 mm×4.6 mm,5μm)was used to detected paracetamol with water(containing 0.5%phosphoric acid and 0.4%triethylamine)-acetonitrile(94∶6)as the mobile phase.The flow rate was 1.0 mL·min^(-1),the detection wavelength was 244 nm,and the column temperature was 30℃.Sepax Amethyst C_(18)-H column(250 mm×4.6 mm,5μm)was used to detected caffeine and chlorpheniramine maleate with water(containing 0.5%phosphoric acid and 0.4%triethylamine)-acetonitrile(93∶7)as the mobile phase.The flow rate was 1.0 mL·min^(-1),the detection wavelength was 264 nm,and the column temperature was 30℃.Welchrom C_(18) column(250 mm×4.6 mm,5μm)was used to detected linarin with methanol-water-glacial acetic acid(26∶23∶1)as the mobile phase.The flow rate was 1.0 mL·min^(-1),the detection wavelength was 334 nm,and the column temperature was 30℃.Results All the 4 components showed good linearity.The average recovery was at 97.08%-104.37%,RSD was at 0.50%-3.8%(n=9).The f value of comprehensive evaluation function of 10 batches compound Ganmaoling granules was between-5.76~-5.26,and RSD was 3.7%.Conclusion The method is accurate and repeatable,which can be used for the determination of 4 components in compound Ganmaoling granules.Comprehensive quality of the 10 batches of samples is stable and controllable.