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目的:首次建立藏药复方二十五味珊瑚丸中酯型生物碱和硫化汞含量测定方法。方法:采用HPLC测定二十五味珊瑚丸中酯型生物碱。硫氰酸盐法测定硫化汞。Phenomenex Luna C18(2)色谱柱(4.6 mm×150 mm,5μm);柱温:35℃;流动相:甲醇-0.05 mol.L-1磷酸二氢钾-醋酸-异丙醇(67∶173∶4∶4);检测波长:230 nm;流速:1.0 mL.min-1。结果:乌头碱线性方程为Y=6.974×105X-28.1,r=0.999 8;表明乌头碱在0.096~0.480μg范围内进样量与峰面积呈良好线性关系。平均回收率为93.1%,RSD为2.1%。结论:该法准确、可靠、重复性好,可有效控制二十五味珊瑚丸中酯型生物碱和硫化汞限量。
Objective: To establish the method for the determination of ester alkaloid and mercuric sulfide in Tibetan medicine coral pills for the first time. Methods: The content of ester alkaloids in twenty-five coral pills was determined by HPLC. Thiocyanate method for the determination of mercuric sulfide. Phenomenex Luna C18 column (4.6 mm × 150 mm, 5 μm); column temperature: 35 ° C .; mobile phase: methanol -0.05 mol.L -1 potassium dihydrogen phosphate-isopropanol (67: 173: 4: 4); detection wavelength: 230 nm; flow rate: 1.0 mL.min-1. Results: The linear equation of aconitine was Y = 6.974 × 105X-28.1, r = 0.999 8. It showed that there was a good linear relationship between the injection volume and peak area of aconitine in the range of 0.096-0.480 μg. The average recovery was 93.1% with a RSD of 2.1%. Conclusion: The method is accurate, reliable and reproducible. It can effectively control the ester alkaloid and mercuric sulfide in Twenty-five coral pills.