蓖麻子中蓖麻碱的提取分离与含量测定

Separation and determination of ricinine from Ricinus Semen

目的：建立蓖麻子中毒性成分蓖麻碱的含量测定方法。方法：采用溶剂提取、硅胶柱层析和重结晶等提取分离手段得到蓖麻碱对照品；采用HPLC法测定蓖麻子中蓖麻碱含量，以依利特Hypersil ODS2（150mm×4．6mm，5p．m）色谱柱为固定相，以水-乙腈-二乙胺（89：11：0．03）为流动相，流速0．8mL·min^-1，检测波长307nm。结果：从400g蓖麻子种皮中分离、纯化得到纯度大于98．5％的蓖麻碱对照品210mg；蓖麻碱在0．1255～2．5100μg范围内，进样量与峰面积之间有良好的线性关系（R^2=1），平均回收率为99．9％；蓖麻子中蓖麻碱含量为0．1695％～0．2396％。结论：所设计的提取分离步骤得到的蓖麻碱纯度高，可作为含量测定用对照品；所建立的含量测定方法简便、快速、重复性好，可用于蓖麻子中毒性成分蓖麻碱的含量测定。

Objective： To establish an analytical method for determination of the toxic compound ricinine from Ricinus Semen. Methods： The ricinine was obtained by solvent extract, silica gel column chromatography and recrystallization. The HPLC analysis was performed on a Hypersil ODS2 column （150 mm× 4.6 mm, 5 μm）, using water-acetonitrile-diethylamine （89：11：0.03） as mobile phase at flow rate of 0.8 mL. min^-1 with detection wavelength of 307 nm. Results： A total of 210 mg of rieinine with the purity over 98.5% was isolated and purified from 400 g of seed coat of Ricinus Semen. Within the test range of 0. 125 5 - 2.510 0 μg, the peak area of ricinine versus injected amounts showed good correlation （R^2 = 1 ） , and mean recovery of the analyte was 99.9%. The contents varied from 0. 169 5% to 0. 239 6% in Ricinus Semen. Conclusion： The ricinine is obtained with high purity and can be used as reference substance. The established HPLC method has proved to be simple, rapid and repeat- able, and can be applied to the determination of rieinine from Ricinus Semen.