高纯度苏丹红单体的高效逆流色谱纯化研究

Purification of High Pure Sudans by High Performance Countercurrent Chromatography

建立了两种高纯度苏丹红单体的高效逆流色谱分离纯化方法。采用1 000 m L逆流色谱分离柱,V(正己烷)∶V(乙腈)=1∶1体系,上相为固定相,下相为流动相,流动相流速为45 m L/min,上样量600 mg,经过一次分离纯化(40 min),即可将苏丹红Ⅱ样品的检测纯度(280 nm下)从97.01%提高到98.42%,得率为90.8%。在254 nm和500 nm下的纯化组分检测纯度也分别可以达到98.01%和99.79%。采用同样的色谱柱,V(正己烷)∶V(乙腈)∶V(乙酸乙酯)=5∶5∶1体系,上相为固定相,下相为流动相,流动相流速为20 m L/min,上样量900 mg,经过两步分离纯化,可以将苏丹红Ⅳ的检测纯度(280 nm下)从84.67%提高到96.6%,得率为48.8%。在254 nm和500 nm下的检测纯度可以分别达到97.16%和98.32%。该方法具有快速、高效、制备量大等特点,可以为高质量苏丹红标准样品的研制提供技术支持。

The separation methods of two high pure Sudans by high performance countercurrent chromatography（ CCC） were developed. The solvent system composed of hexane： acetonitrile（ 1∶ 1,V / V） with the lower phase was the mobile phase at the flow-rate of 45 m L / min,and 600 mg sudan Ⅱ sample was purified within 40 min using the 1 000 m L column. The results showed that its purity（ 280 nm） was improved from 97. 01% to 98. 42% with the yield of 90. 8%,while its purity at 254 nm and 500 nm reached 98. 01% and 99. 79%,respectively. Using the solvent system composed of hexane∶ acetonitrile∶ethyl acetate（ 5∶ 5∶ 1,V / V / V） with the lower phase as the mobile phase at the flow-rate of 20 m L / min,900 mg Sudan Ⅳ sample was purified through two-steps. As a result,its purity（ 280 nm） could be improved from 84. 67% % to 96. 6% with the yield of 48. 8%,while its purity at 254 nm and 500 nm could also reach 97. 16% and 98. 32%,respectively. This method with the characters of high-speed,high-efficiency,and high preparation quality could give supports for the study of high pure Sudans standards.