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目的:优化和提高复方小儿止咳口服溶液的质量标准。方法:采用薄层色谱法(TLC)对制剂中的甘草进行定性鉴别;采用化学反应法对制剂中吐根酊、氯化铵进行定性鉴别;采用高效液相色谱法(HPLC)测定制剂中甘草酸铵的含量:色谱柱为Agilent Zorbax XDB C18,流动相为乙腈-0.2 mol/L乙酸铵溶液(20 ∶ 80,V/V),流速为1.0 ml/min,检测波长为250 nm,柱温为30 ℃,进样量为10 μl。结果:甘草的TLC斑点清晰,分离良好,阴性对照无干扰。吐根酊、氯化铵的鉴别反应阳性特征显著。甘草酸铵检测质量浓度线性范围为6.08~72.96 μg/ml(r=0.999 9);精密度、稳定性、重复性试验的RSD<1.0%;加样回收率为99.69%~100.28%(RSD=0.20%,n=6)。结论:经优化和提高的标准可有效控制复方小儿止咳口服溶液的质量。
OBJECTIVE: To optimize and improve the quality standard for Compound pediatric anticough oral solution. METHODS: TLC was adopted for the qualitative identification of Glycyrrhiza uralensis; chemical reaction was adopted for the qualitative identification of ipecac tincture, ammonium chloride; and HPLC was adopted for the content determination of ammonium glycyrrhizinate: the column was Agilent Zorbax XDB C18 with mobile phase of acetonitrile-0.2 mol/L ammonium acetate (20 ∶ 80,V/V) at a flow rate of 1.0 ml/min, the detection wavelength was 250 nm, column temperature was 30 ℃, and the injection volume was 10 μl. RESULTS: TLC spots of G. uralensis were clear and well-separated, negative control without interference. Differential response of ipecac tincture and ammonium chloride showed significant positive characteristics. The linear range of ammonium glycyrrhizinate was 6.08-72.96 μg/ml (r=0.999 9); RSDs of precision, stability and reproducibility tests were lower than 1.0%; recovery was 99.69%-100.28% (RSD=0.20%,n=6). CONCLUSIONS: Optimizing and improving the standard are helpful for the quality control of Compound pediatric anticough oral solution.
复方小儿止咳口服溶液质量标准薄层色谱法高效液相色谱法
Compound pediatric anticough oral solutionQuality standardTLCHPLC
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