Department of Chemical Engineering, National Chung Hsing University, 250, Kuo-Kuang Road, Taichung 402, Taiwan.
J Chromatogr A. 2012 Dec 28;1270:1-8. doi: 10.1016/j.chroma.2012.10.036. Epub 2012 Oct 23.
This work investigated column elution chromatography coupled with supercritical anti-solvent precipitation to produce carotenoid rich microsized particulates from microalgal Dunaliella salina species. The extract contained carotenoids ranging from 61.3 mg/g(salina) to 72.5 mg/g(salina) using ultrasonic stirred ethyl ether or tetrahydrofuran (THF) extraction. When 10 L of ethyl alcohol was employed to elute the THF extract, purity of trans-β-carotene is 823.6 mg/g with a recovery of 86.2%. It was found that the supercritical anti-solvent of THF solution at 160 bar and 318 K produced powdered particulates with a purity of carotenoids above 90%. Subsequently, a central composite response surface design method was used to design supercritical anti-solvent precipitation of carotenoid-rich THF solution. This was accomplished by increasing the pressure from 140 bar to 180 bar and the time from 40 min to 60 min at a feed flow rate of 0.2 mL/min. A CO(2) flow rate of 15 L/min and a temperature of 318 K were also used to determine the effects on purity and recovery of trans-β-carotene. The combined process produced micronized precipitates with a mean particle size ranging from 3.5 μm to 19 μm and the purity of trans-β-carotene attained was 926.8 mg/g with a recovery of 54%.
本工作研究了柱洗脱色谱法与超临界抗溶剂沉淀相结合，从微藻杜氏盐藻中制备富含类胡萝卜素的微颗粒。使用超声搅拌乙醚或四氢呋喃 (THF) 提取，提取物中的类胡萝卜素含量范围为 61.3mg/g(salina)至 72.5mg/g(salina)。当使用 10L 乙醇洗脱 THF 提取物时，反式-β-胡萝卜素的纯度为 823.6mg/g，回收率为 86.2%。结果发现，THF 溶液在 160 巴和 318K 的超临界抗溶剂条件下生成的粉末状颗粒中类胡萝卜素的纯度超过 90%。随后，采用中心组合响应面设计方法设计了富含类胡萝卜素的 THF 溶液的超临界抗溶剂沉淀。通过将压力从 140 巴提高到 180 巴，将时间从 40 分钟延长到 60 分钟，同时保持进料流速为 0.2mL/min 来实现这一目标。还使用 CO(2)流速为 15L/min 和温度为 318K 来确定其对反式-β-胡萝卜素的纯度和回收率的影响。该联合工艺生产的微米级沉淀物的平均粒径范围为 3.5μm 至 19μm，反式-β-胡萝卜素的纯度达到 926.8mg/g，回收率为 54%。
