复方薄荷酚酸酊的质量标准研究

Study on the quality standards of Fufangbohefensuan tincture

目的:建立复方薄荷酚酸酊的质量标准。方法:采用薄层色谱法(TLC)鉴别复方薄荷酚酸酊中的薄荷脑,蒸馏法测定乙醇的含量,酸碱滴定法测定硼酸的含量。采用HPLC法测定苯酚和地塞米松磷酸钠的含量,色谱柱为Agilent Zorbax SB C18柱(250mm×4.6mm,5μm);流动相:0.05mol/L乙酸钠溶液(用冰乙酸调节pH至4.0)-甲醇(40∶60);检测波长:242nm;进样量:20μl;流速:1.0ml/min;柱温:30℃。结果:TLC鉴别斑点清晰,分离效果良好,阴性对照无干扰。样品中乙醇的含量范围为42%~52%。酸碱滴定法终点敏锐,准确度高,操作简便。苯酚、地塞米松磷酸钠分别在502~1506、5.61~89.63μg/ml范围内线性关系良好(r=0.9999),平均加样回收率分别为(99.4±0.36)%和(100.1±0.29)%(n=3)。结论:该方法简便、可靠,可用于复方薄荷酚酸酊的质量控制。

Objective : To establish the quality standards of Fufangbohefensuan tincture.Methods: Menthol in Fufangbohefensuan tincture was identified by thin layer chromatography(TLC) method.The contents of ethanol and boric acid in Fufangbohefensuan tincture were determined by distillation and acid-base titration,respectively.The contents of phenol and dexamethasone sodium phosphate were determined by HPLC method with Agilent Zorbax SB C 18 column (250 mm×4.6 nm,5 μm ) as the chromatographic column.The mobile phase consisted of 0.05 mol/L sodium acetate solution(the pH value was adjusted to 4.0 with glacial acetic acid)-methanol (40∶60).The detection wavelength was 242 nm and the injection volume was 20 μl.The flow rate was 1.0 ml/min and the column temperature was 30 ℃.Results: The spots were clear,the specificity was good and the negative control had no interference in TLC detection.The contents of phenol in the sample ranged from 42% to 52%.Acid-base titration method had sharp end point,high accuracy and was easy to operate.The contents of phenol and dexamethasone sodium phosphate in the ranges of 502-1506 and 5.61-89.63 μg/ml showed a good linear relationship ( r =0.999 9).The average recovery rates of phenol and dexamethasone sodium phosphate were (99.4±0.36)% and (100.1±0.29)%( n =3).Conclusion: The established method is simple and reliable,and could be used for quality control of Fufangbohefensuan tincture.