克咳片中8个成分的含量测定

目的： 建立同时测定克咳片中8个成分含量的方法。方法： 采用高效液相色谱-二极管阵列检测（HPLC-DAD）法。色谱柱：Agilent ZORBAX Eclipse Plus C₁₈（5 μm，250 mm×4.6 mm）；流动相：乙腈（A）-0.05%磷酸水溶液（B），梯度洗脱；流速：0.7 mL·min^-1；检测波长：210 nm（吗啡、盐酸麻黄碱、盐酸伪麻黄碱、磷酸可待因、苦杏仁苷）、237 nm（甘草苷、甘草次酸）、251 nm（甘草酸铵）；柱温：30℃；进样量：10 μL。采用统计分析软件对含量测定结果进行主成分分析与聚类分析。结果： 吗啡、盐酸麻黄碱、盐酸伪麻黄碱、磷酸可待因、苦杏仁苷、甘草苷、甘草酸铵和甘草次酸检测质量浓度线性范围分别为7.895~157.9、9.405~188.1、10.07~201.4、0.860 5~17.21、0.556 5~11.13、2.950~59.01、13.24~264.9、6.595~131.9 μg·mL^-1（r ≥ 0.999 1）；定量下限分别为1.215、1.323、0.951、0.674、0.509、0.912、1.134、0.856 μg·mL^-1；精密度、稳定性（48 h）、重复性试验的RSD<2.0%（n=6或n=7）；平均加样回收率分别为98.4%、98.7%、98.5%、97.6%、97.7%、98.6%、98.6%、98.4%（n=9）；12批样品存在一定差异，主要是麻黄、罂粟壳和甘草投料造成。结论： 本法简便、准确，重复性好，提示厂家在生产过程中要加强对麻黄、罂粟壳和甘草质量的控制，可为克咳片质量提高提供参考。

Objective: To establish a method for simultaneous determination of 8 constituents in Keke tablets.Methods: HPLC-DAD analysis was performed on Agilent ZORBAX Eclipse Plus C₁₈(250 mm×4.6 mm,5 μm)with the column temperature of 30℃ and the injection volume was 10 μL.The mobile phase was acetonitrile(A)-0.05% phosphoric acid (B)with gradient elution at the flow rate of 0.7 mL·min^-1 and the detection wavelength was 210 nm for morphine,ephedrine hydrochloride,pseudoephedrine hydrochlorid,phosphate codeine and amygdalin;237 nm for liquiritin and glycyrrhetinic acid;251 nm for ammonium glycyrrhizate. The principal component analysis and cluster analysis were conducted for the results of content determination by statistical software.Results: The linear ranges were 7.895-157.9 μg·mL^-1 for morphine,9.405-188.1 μg·mL^-1 for ephedrine hydrochloride,10.07-201.4 μg·mL^-1 for pseudoephedrine hydrochlorid,0.860 5-17.21 μg·mL^-1 for phosphate codeine,0.556 5-11.13 μg·mL^-1 for amygdalin,2.950-59.01 μg·mL^-1 for liquiritin,13.24-264.9 μg·mL^-1 for ammonium glycyrrhizate,3.149-62.98 μg·mL^-1 for glycyrrhetinic acid,respectively.The limits of quantitation were 1.215,1.323,0.951,0.674,0.509,0.912,1.134,0.856 μg·mL^-1,with r ≥ 0.999 1.RSDs of precision,reproducibility and stability tests(48 h) were lower than 2.0%(n=6 or n=7).Average recoveries were 98.4%,98.7%,98.5%,97.6%,97.7%,98.6%,98.6%,98.4%(n=9).There were some differences among 12 batches of sample,mainly due to different dosages of Ephedrae Herba,Papaveris Pericarpium and Radix Glycyrrhiza.Conclusion: The method is simple and accurate with good repeatability.It is suggested that the quality control of Ephedrae Herba,Papaveris Pericarpium and Glycyrrhizae Radix et Rhizoma should be strengthed in the process of production for providing a reference of Keke tablets quality improvement.

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