苍术中非法添加硫酸阿托品及氢溴酸东莨菪碱的检测方法

Study on Determination of Atropine Sulfate and Scopolamine Hydrobromide Illegally Added to Atractylodes

目的建立中药苍术中非法添加硫酸阿托品及氢溴酸东莨菪碱的定性定量检测方法。方法采用薄层色谱法定性、高效液相色谱法定量;色谱柱为phenomenex Luna C18柱(200 mm×4.6 mm,5μm),流动相为0.07 mol/L磷酸钠溶液(含0.017 5 mol/L十二烷基硫酸钠,用磷酸调节pH至6.0-乙腈(70∶30),流速为1.0 mL/min,柱温为30℃,检测波长为216 nm。结果硫酸阿托品及氢溴酸东莨菪碱进样量分别在1.97～9.85μg和2.03～10.15μg的范围内与峰面积积分值线性关系良好,平均加样回收率分别为99.67%和99.77%,RSD为0.12%和0.19%(n=6)。结论该方法简便、快速、准确,可用于检测苍术中非法添加的硫酸阿托品及氢溴酸东莨菪碱。

Objective To establish TLC and HPLC methods for the determination of atropine sulfate and scopolamine hydrobromide illegally added to atractylodes.Methods The TLC and HPLC methods were used for qualitative and quantitative determination respectively.Phenomenex Luna C18 column（200 mm × 4.6 mm,5 μm） was taken as chromatographic column.The mobile phase was composed of acetonitrile-0.07 mol /L sodium phosphate solution（containing 0.017 5 mol /L sodium dodecyl sulfate,using phosphoric acid to adjust pH value to 6.0,30 ∶ 70）,the flow rate was 1.0 mL /min,the column temperature was 30 ℃,the detection wavelength was 216 nm.Results Atropine sulfate and scopolamine hydrobromide had good linearity（r = 0.999 9） in the range of 1.97-9.85 μg and 2.03-10.15 μg respectively.The average recovery rates were 99.67% and 99.77%,RSD = 0.12% and 0.19% respectively.Conclusion The method is rapid,simple and accurate,which can be applied to determine atropine sulfate and scopolamine hydrobromide illegally added to atractylodes.