颠茄流浸膏真伪鉴别及含量测定方法研究

目的:对颠茄流浸膏进行定性定量研究,鉴别真伪,提高颠茄流浸膏的质量标准。方法:运用薄层色谱法对颠茄流浸膏进行定性分析;采用高效液相色谱法测定硫酸天仙子胺的含量,色谱柱为Shim-pack VP-ODS(4.6 mm×250 mm,5μm)柱,流动相为0.004%磷酸溶液(含0.25%十二烷基硫酸钠)-乙腈(60∶40),流速1.0 mL.min-1,检测波长210 nm,柱温30℃。结果:薄层色谱方法能有效识别非法添加硫酸阿托品,鉴别特征明显,专属性强;硫酸天仙子胺进样量在0.2888～16.50μg范围内线性良好(r=1.000),平均回收率为103.8%(RSD=1.6%,n=6)。结论:本方法专属性强、灵敏度高、操作简便,对30余批不同生产企业颠茄流浸膏进行鉴别和含量测定,结果有6批次样品检出非法添加硫酸阿托品,该方法可为颠茄流浸膏的质量控制提供依据。

Study on identification and content determination of Extractum Belladonnae Liquidum

Objective: To establish qualitative and quantitative methods for the quality evaluation of Extractum Belladonnae Liquidum.Methods: Extractum Belladonnae Liquidum was identified with TLC method.The separation and determination of hyoscyamine sulfate were obtained by RP-HPLC,with Shim-pack VP-ODS column(4.6 mm × 250 mm,5 μm) as analytical column and 0.004% phosphoric acid solution(containing 0.25% dodecyl sulfonate sodium salt)-acetonitrile(60∶ 40) as the mobile phase.The flow rate was 1.0 mL.min-1 at 30 ℃,and the detection wavelength was at 210 nm.Results: The identification of TLC was characteristic and specific to figure out atropine sulfate which was illegally added into Extractum Belladonnae Liquidum.Calibration curve of hyoscyamine sulfate showed good linear regression(r = 1.000) within the test ranges of 0.2888-16.50 μg;Average recovery was 103.8%(RSD = 1.6%,n = 6).Conclusion: The methods were proved to be sensitive,reliable and useful by analyzing thirty different samples of Extractum Belladonnae Liquidum.Atropine sulfate was detected in six samples.These methods have been successfully applied to evaluate the quality of Extractum Belladonnae Liquidum.