颠茄草的质量标准提升

Improvement on Quality Standard of Belladonnae Herba

目的:针对颠茄草的现行标准较低且缺项的问题,对颠茄草的质量标准进行提高。方法:以东莨菪内酯、硫酸阿托品、硫酸天仙子胺为对照品,以乙酸乙酯-甲醇-浓氨试液(17∶4∶2)为展开剂,采用薄层色谱法对颠茄草进行定性鉴别;按2020年版《中华人民共和国药典》(四部)通则相关方法对颠茄草的水分、总灰分和醇溶性浸出物进行测定;采用高效液相色谱法(HPLC)测定颠茄草中硫酸天仙子胺和氢溴酸东莨菪碱的含量,流动相选择乙腈-54 mmol·L^(-1)磷酸盐缓冲液(14∶86),流速1.0 mL·min^(-1),检测波长210 nm。结果:薄层色谱图中斑点清晰、分离度好、专属性强;硫酸天仙子胺和氢溴酸东莨菪碱分别在0.0247~0.7896 g·L^(-1)(r=0.9999),0.0039~0.1240 g·L^(-1)(r=0.9999)与峰面积呈良好线性关系,平均加样回收率分别为100.29%(RSD 1.6%),99.04%(RSD 1.4%);拟定水分不得过13.0%,总灰分不得过13.0%,醇溶性浸出物不得少于10.0%;鉴于氢溴酸东莨菪碱含量较低且变异范围大,拟定硫酸天仙子胺质量分数不得少于0.098%。结论:建立的方法操作简便、专属性强、重复性好,可用于提升颠茄草的质量控制标准。

Objective:To improve the current standard of Belladonnae Herba in the 2020 edition of Chinese Pharmacopoeia.Method:Taking hyoscyamine sulfate,atropine sulfate and scopoletin as reference substances,and ethyl acetate-methanol-concentrated ammonia(17∶4∶2)as developing solvent,thin layer chromatography(TLC)was applied in the qualitative identification of Belladonnae Herba.The moisture,total ash and ethanol-soluble extract of Belladonnae Herba were determined based on the general principles in the 2020 edition of Chinese Pharmacopoeia(volumeⅣ).The contents of hyoscyamine sulfate and scopolamine hydrobromide were analyzed by high performance liquid chromatography(HPLC)with mobile phase of acetonitrile-54 mmol·L^(-1)phosphate buffer solution(14∶86),flow rate of 1.0 mL·min^(-1) and detection wavelength at 210 nm.Result:The spots in the TLC were clear with good separation and specificity.Hyoscyamine sulfate and scopolamine hydrobromide showed a good linearity with peak area in the range of 0.0247-0.7896 g·L^(-1)(r=0.9999)and 0.0039-0.1240 g·L^(-1)(r=0.9999),the average recoveries of these two ingredients were 100.29%(RSD 1.6%)and 99.04%(RSD 1.4%),respectively.The limits for moisture,total ash in Belladonnae Herba should be less than 13.0%and the limit for the ethanol-soluble extract should be more than 10.0%.Due to the low content and wide variation of scopolamine hydrobromide,the content of hyoscyamine sulfate should not be less than 0.098%.Conclusion:The established method is simple,specific and reproducible,which can be used to improve the quality control standard of Belladonnae Herba.