安痛舒贴质量标准研究

Quality Standard of Antongshu Plaster

目的建立安痛舒贴的质量标准。方法采用薄层色谱法定性鉴别姜黄、甘遂,采用高效液相色谱法测定马钱子和当归含量。马钱子含量测定,Ultimate C_(18)色谱柱、Capcell Pak C_(18) MG柱(250 mm×4.6 mm,5μm),乙腈-0.01 mol/L磷酸二氢钾与0.02 mol/L庚烷磺酸钠等量混合溶液(用磷酸调pH至2.8)(20∶80)为流动相,流速为1.0 m L/min,柱温为35℃,检测波长为260 nm。当归含量测定,色谱柱同上,甲醇-0.05 mol/L磷酸溶液(26∶74)为流动相,检测波长为319 nm,柱温为35℃。结果士的宁进样量在0.024 92~0.438 4μg、马钱子碱进样量在0.023 92~0.478 4μg、阿魏酸进样量在0.089 2~0.802 8μg范围内,与峰面积线性关系良好;回归方程分别为Y=5.598 24×10~6X+77 520(r=0.999 9)、Y=6×10^(-7) X+0.007 5(r=0.999 8)、Y=6×10^(-2) X+0.563 87(r=0.999 8),平均加样回收率马钱子碱为99.97%,士的宁为96.87%,阿魏酸为97.68%(n=6)。结论该质量标准操作简便易行,定性、定量方法准确度高、重复性好,检测设定指标合理,可用于安痛舒贴的质量控制。

Objective To establish the quality standard for the Antongshu Plaster. Methods TLC was used for the qualitative identification of Curcuma longa,Euphorbia kansui,HPLC was used for the content determination of Strychnos nux-vomica and Angelica sinensis. The content determination of Strychnos nux-vomica： Ultimate C_（18） column and Capcell Pak C_（18） MG column（ 250 mm × 4. 6 mm,5 μm） were adopted with acetonitrile-0. 01 mol/L KH_2PO_4 and 0. 02 mol/L sodium heptanesulfonate mixture solution（ pH = 2. 8adjusted with phosphoric acid）（ 20 ∶ 80） as the mobile phase,the flow rate of 1. 0 m L/min,the column temperature was 35 ℃,the detection wavelength was 260 nm. The content determination of Angelica sinensis： The column was the same as above,the mobile phase was methanol-0. 05 mol/L phosphoric acid solution（ 26 ∶ 74）,the detection wavelength was 319 nm,the column temperature was 35 ℃.Results The strychnine,brucine and ferulic acid showed a good linear in the range of 0. 024 92-0. 438 4 μg,0. 023 92-0. 478 4 μg,0. 089 2-0. 802 8 μg,respectively,and the regression equations were Y = 5. 598 24 × 10-6 X ＋ 77 520（ r = 0. 999 9）,Y = 6 × 10-（-7） X ＋0. 007 5（ r = 0. 999 8）,Y = 6 × 10-（-2） X ＋ 0. 563 87（ r = 0. 999 8）,respectively. The average recovery rate of brucine,strychnine and ferulic acid were 99. 97 %,96. 87 % and 97. 68 %,respectively. Conclusion The quality standard is simple and easy to operate. The qualitative and quantitative methods have high accuracy,good repeatability and reasonable test setting index,which can be used for the quality control of Antongshu Plaster.