重结晶法提纯番茄红素的研究

Research on Purifying Lycopene by Recrystallization

以6%番茄红素油树脂为原料,用重结晶法制备出番茄红素晶体,考察了温度、皂化时间、不同溶剂和重结晶级数对得率及纯度的影响。结果表明,用正己烷作分散剂、无水乙醇作助剂,在70℃条件下皂化60min,水洗正己烷层至中性,真空挥去部分溶剂,冷却滤出番茄红素晶体溶于65℃乙酸乙酯中至饱和,缓慢降温至0℃析出晶体。对样品紫外、红外扫描得到的色谱图具有典型的特征峰,重结晶3次样品HPLC分析保留时间与标准品一致,所得样品为全反式番茄红素,HPLC法测纯度达104.03%,差示扫描量热法分析纯度达99.17%,总得率为24.7%。本研究为高纯度番茄红素的获得提供了一条有效途径。

Crystal of lycopene was prepared by recrystallization when a content of 6% lycopene oleoresin was used as raw material. Effect of temperature, time of saponification, solvent and order of recrystallization on yield and purity of lycopene was carried out. Results showed that the preparation process was as follows： when hexane and ethanol were used as scattering and aid agents respectively, the raw material was saponified 60 rain at 70℃, and hexane was washed until neutral; and then the raw material was cooled and filtered after some solvent was evaporated at vacuum condition; after that it dissolved in ethyl acetate at 65℃ until saturates; finally the crystal can be produced when it was cooled slowly till 0℃. Mass spectrogram by UV-scan and infrared spectrophotometry of prepared lycopene sample had typical peaks. The retention time of sample after 3 times of recrystallization was the same as that of standard sample by HPLC. The lycopene prepared was proved to be all-trans conformation. Its purities were 104.03% and 99.17% by HPLC and DSC analysis, respectively. Its total yield was 24.7%. The research has provided a useful method for obtaining high purity lycopene.