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目的:从白芥子中分离制备芥子碱,并采用高效液相色谱法(HPLC)测定其纯度。方法:白芥子粉碎,脱脂,醇提取后,硫氰酸钾析晶,以乙醇与水多次交互重结晶。HPLC柱为ZORBAXSB-Aq柱(4.6mm×250mm,5μm),流动相为乙腈-0.08mol/LKH2P04溶液(20:80),流速为1.0ml/min,检测波长326nm,柱温25℃。结果:制得芥子碱硫氰酸盐呈浅黄色针状结晶,得率为0.82%,RP-HPLC法检测其纯度达95.12%。结论:采用本溶剂萃取法制备芥子碱,以其纯度高、得率较高、方法简便的优点,可适用于工厂产业化生产。
OBJECTIVE: To prepare and prepare the sinapine from the seeds of Brassica chinensis by high performance liquid chromatography (HPLC). Methods: The seeds of white mustard were crushed, defatted and extracted with alcohol. The potassium thiocyanate was crystallized and recrystallized with ethanol and water several times. The HPLC column was a ZORBAXSB-Aq column (4.6 mm×250 mm, 5 μm), the mobile phase was acetonitrile-0.08 mol/L KH2P04 solution (20:80), the flow rate was 1.0 ml/min, the detection wavelength was 326 nm, and the column temperature was 25° C. Results: The sinapine thiocyanate was obtained as pale yellow needles with a yield of 0.82%. The purity of sulfonation by RP-HPLC was 95.12%. Conclusion: The preparation of sina alkaloids by the solvent extraction method has the advantages of high purity, high yield and simple method, which can be applied to the industrial production of the plant.