摘要
目的建立玉龙贴膏的质量标准。方法采用薄层色谱法鉴别方中赤芍、肉桂。采用高效液相色谱法测定芍药苷的含量和乌头碱的限量,色谱柱为XTerra RP18柱(250 mm×4. 6 mm,5μm);芍药苷含量测定的流动相为甲醇-0. 05 mol/L磷酸二氢钾溶液(40∶65),流速为1. 0 m L/min,检测波长为230 nm;乌头碱限量检查的流动相为甲醇-0. 1%三乙胺(70∶30),流速为1. 0 m L/min,检测波长为235 nm。结果薄层色谱鉴别斑点清晰,阴性对照无干扰,专属性强,重复性良好;芍药苷进样量在0. 515~10. 300μg范围内与峰面积线性关系良好(r=0. 999 2),平均回收率为98. 35%,RSD为0. 94%(n=6);乌头碱进样量在0. 301 2~3. 012 0μg范围内与峰面积线性关系良好(r=0. 999 0),平均回收率为97. 87%,RSD为1. 13%(n=6)。结论建立的定性定量方法简便、可靠、准确,可作为玉龙贴膏的质量控制标准。
Objective To establish the quality standard of Yulong Plaster. Methods Radix Paeoniae Rubra and Cortex Cinnamomi were identified by TLC mtthod. The content of peoniflorin and limit examination of aconitine were determined by HPLC method. The chromatographic column was XTerra RP18 column( 250 mm × 4. 6 mm,5 μm). The mobile phase of peoniflorin consisted of methanol-0. 05 mol/L monopotassium phosphate solution( 40∶ 65),the flow rate was 1. 0 m L/min,and the detection wavelength was 230 nm. The mobile phase of aconitine consisted of methanol-0. 1% triethylamine( 70∶ 30),the flow rate was 1. 0 m L/min,and the detection wavelength was 235 nm. Results The TLC method had clear spots, strong specificity and good repeatability, the negative control had no interference. Peoniflorin showed a good linear relationship within the range of 0. 515-10. 300 μg( r = 0. 999 2),the average recovery rate was 98. 35%,and the RSD was 0. 94%( n = 6). Aconitine showed a good linear relationship within the range of 0. 301 2-3. 012 0 μg( r = 0. 999 0), the average recovery rate was 97. 87% and RSD was 1. 13%( n = 6). Conclusion The established qualitative and quantitative methods are simple,reliable and accurate,which can be used for the quality control of Yulong Plaster.
引文
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