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目的:采用BBD-响应面法优化黑果枸杞色素的渗漉法提取工艺,并对其纯化工艺进行研究。方法:采用单因素实验结合BBD-响应面法,对影响渗漉法提取的3个主要因素乙醇浓度、渗漉速度、溶剂倍数进行了优化。通过筛选出吸附性能最好的大孔树脂,对影响其吸附与解析的因素:上样液浓度、上样液pH值、径高比、上样流速、水洗用量、洗脱剂浓度、洗脱剂pH值、洗脱剂流速进行考察,并对色素色价和产率进行测定。结果:最佳工艺是采用pH3.0,20倍量79%乙醇,以1 mL/min的流速进行渗漉提取。采用X-5大孔树脂纯化色素,径高比1:15、色素液浓度0.02 g/mL,上样液pH3.0、上样量90 mL,流速3 mL/min为最佳吸附条件;以5 BV的95%乙醇在pH2.0、流速3 mL/min的条件下洗脱效果最佳,纯化色素产率可达7.33%,色价为21.7,重复性较好,适合于工业化生产。结论:该工艺操作简单、重复性好,节约成本,可为色素大工业生产提供参考。
OBJECTIVE: To optimize the extraction process of perilla pigment of Lycium barbarum by BBD-response surface methodology and to study its purification process. Methods: The single factor experiment combined with BBD-response surface method was used to optimize the three main factors influencing the percolation method: ethanol concentration, percolation rate and solvent multiples. By screening out the best macroporous resin adsorption factors on the adsorption and analysis of the factors: the concentration of the sample, the pH value of the sample, diameter and height ratio, the sample flow rate, the amount of water washing, eluent concentration, elution PH value, eluent flow rate were investigated, and the pigment color value and yield were determined. Results: The optimum process was percolation extraction with a flow rate of 1 mL / min using 20% 79% ethanol at pH3.0. X-5 macroporous resin was used to purify the pigment. The optimum conditions were as follows: diameter-to-height ratio 1:15, dye solution concentration 0.02 g / mL, sample solution pH 3.0, sample volume 90 mL and flow rate 3 mL / 95% ethanol of 5 BV has the best elution efficiency at pH2.0 and flow rate of 3 mL / min. The yield of purified pigment is up to 7.33%, the color value is 21.7, and the repeatability is better. It is suitable for industrial production. Conclusion: The process is simple, good repeatability, cost savings, can provide a reference for the large industrial production of pigment.