目的:建立高效液相色谱法测定感冒灵颗粒和复方感冒灵颗粒中对乙酰氨基酚、咖啡因和马来酸氯 苯那敏含量。方法:采用 Inertsil ODS-3(250 mm×4.6 mm,5 μm)色谱柱,流动相为乙腈和磷酸盐缓冲液(取磷酸二氢铵 11.5 g,加水溶解并稀释至 1 000 mL,加磷酸 1.0 mL,混匀),梯度洗脱,流速 1.0 mL·min-1,检测波长 264 nm,由于制剂中对乙酰氨基酚的含量远大于咖啡因和马来酸氯苯那敏,供试品溶液分别进样 5 μL和 100 μL。结果:对乙酰氨基酚、咖啡因和马来酸氯苯那敏的分离度良好;上述 3 个成分的质量浓度分别在 0.131 7~1.185、0.010 38~0.093 42、0.001 802~0.016 22 mg·mL-1 范围内,线性关系良好,相关系数(r2)均为 0.999 9;稳定性和重复性试验的 RSD 均小于 2.0%;感冒灵颗粒中 3 个成分的平均回收率(n=9)分别为 100.6%、100.0% 和 100.1%,复方感冒灵颗粒中 3 个成分的平均回收率(n=9)分别为 101.0%、100.3% 和 101.0%;3 批感冒灵颗粒中 3 个成分的平均含量(n=2)分别为 104.2%~109.0%、96.0%~96.5% 和 101.2%~105.5%;复方感冒灵颗粒中 3 个成分的平均含量(n=2)分别为 11.403、0.806 和 0.193 mg·g-1。结论:本文建立的 HPLC 法操作简便,稳定性和重复性好,回收率高,可用于感冒了颗粒和复方感冒灵颗粒的含量测定。
Objective:To establish a high performance liquid chromatography method for the determination of paracetamol,caffine and chlorphenamine maleate in Ganmaoling granules and compound Ganmaoling granules. Methods:HPLC experiment was performed on an Inertsil ODS-3 column(250 mm×4.6 mm,5 μm).The mobile phase consisted of acetonitrile and phosphate buffer solution(dissolve 11.5 g of ammonium dihydrogen phosphate in 1 000 mL of water,add 1.0 mL of phosphoric acid)with gradient elution at a flow rate of 1.0 mL·min-1.The detection wavelength was set at 264 nm.Since the content of paracetamol was higher than that of caffeine and chlorpheniramine maleate in the formulation,the injection volumes were 5 μL and 100 μL,respectively. Results:The results showed that the separation of paracetamol,caffeine and chlorpheniramine maleate was good.The linear ranges of paracetamol, caffeine and chlorpheniramine maleate were 0.131 7-1.185,0.010 38-0.093 42 and 0.001 802~0.016 22 mg· mL-1,respectively,the corresponding linear correlation coefficients were all 0.999 9.The RSDs of stability and repeatability tests were less than 2.0%.The average recoveries of Ganmaoling granules were 100.6 %,100.0% and 100.1%(n=9),and the average recoveries of compound Ganmaoling granules were 101.0 %,100.3% and 101.0%(n=9),respectively.The contents(n=2)of paracetamol,caffine and chlorphenamine maleate in Ganmaoling granules were 104.2%-109.0%,96.0%-96.5% and 101.2%-105.5%,and the contents(n=2)of paracetamol,caffine and chlorphenamine maleate in compound Ganmaoling granules were 11.403,0.806 and 0.193 mg·g-1,respectively. Conclusion:The HPLC method is simple with high recovery,good precision and stability, and the method is applied successfully to determine paracetamol,caffeine and chlorpheniramine maleate in Ganmaoling granules and compound Ganmaoling granules.
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