白芥子中芥子碱的制备及纯度测定

Preparation and purity determination of sinapine from seeds of Brassica alba

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：Preparated from seeds of Brassica alba, Sinapine was determinated by RP-HPLC. Methods： Seeds of Brassica alba were shattered, defatted by ether, extracted by alcohol, and crystallized by potassium thiocyanate, then ethanol and water were used to recrystallize for several times. The determination was performed by reversed-phase high performance liquid chromatography（RP-HPLC）, using ZORBAX SB-Aq column 4.6 mm×250 mm, 5 μm. The mobile phase consisted of acetonitrile-0.08 mol/L KH2P04 （20：80） at a flow rate of 1.0 ml/min, and the detection wavelength was 326 nm. Results： Pale yellow needle-like sinapine crystal was obtained, and the yield rate was 0.82%. The purity of sinapine thiocyanate crystal was over 95%. Conclusion： Preparation sinapine by this solvent extraction method was simple, high-purity, high yield, and could be used for industrial production.