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目的:建立反相高效液相色谱法同时测定腰痛宁贴膏中士的宁和马钱子碱含量。方法:色谱柱Intersil C8-3(4.6mm×250 mm,5μm),流动相甲醇-水-冰乙酸(20∶96∶7,用三乙胺调pH为3.10),流速1.0 mL.min-1,检测波长254 nm,柱温30℃。结果:士的宁在0.020 6～0.123 4μg线性关系良好(r=0.999 8),测得平均加样回收率(n=9)为100.28%,RSD1.33%;马钱子碱在0.013 8～0.083 0μg线性关系良好r,=0.999 9,测得平均加样回收率(n=9)为99.82%,RSD 0.84%。结论:方法灵敏、准确、可用于腰痛宁贴膏中士的宁和马钱子碱的质量控制。
Objective: To establish a reversed-phase high performance liquid chromatography method for simultaneous determination of strychnine and brucine in Yaotongning plaster. Method: Column Intersil C8-3 (4.6 mm×250 mm, 5 μm), mobile phase methanol-water-glacial acetic acid (20:96:7, pH adjusted to 3.10 with triethylamine), flow rate 1.0 mL.min-1 The detection wavelength was 254 nm and the column temperature was 30°C. Results: The linear relationship of strychnine was good at 0.020 6-0.123 4 μg (r=0.999 8). The average recovery (n=9) was 100.28%, RSD 1.33%, and brucine at 0.013 8～ 0.083 0 μg good linearity r, = 0.999 9, measured average sample recovery (n = 9) was 99.82%, RSD 0.84%. Conclusion: The method is sensitive, accurate, and can be used for the quality control of losarine and strychnine in Yaotongning plaster.