大孔吸附树脂纯化制备京尼平苷酸的研究

Purification and preparation of geniposidic acid by macroporous resin

研究了大孔吸附树脂从栀子黄色素生产废液的京尼平苷碱水解液中纯化制备京尼平苷酸(GPA)的影响因素及工艺条件,比较了大孔吸附树脂对GPA的脱色、吸附及解吸附性能,确定了最佳制备工艺。结果表明,弱极性DA201树脂的脱色效果较好,且对GPA的吸附性差;非极性树脂DA201C对GPA的吸附率、解吸率较高,分别达到88.7%、98%。在树脂用量1 g/25 m L 10 mg/m L GPA粗提液稀释液、p H 4.0、25℃、120 r/min振荡6 h的条件下,DA201树脂的脱色率为85.9%,GPA保留率为92.3%。DA201C树脂高效吸附GPA的条件为10 mg/m L脱色液、p H3.0、上样速度1 BV/h、上样量7.2 BV。经25%乙醇溶液洗脱、干燥,制备的GPA纯度达到95.1%,回收率为86.2%。上述结果表明,在GPA的分离纯化中,DA201适用于脱色,DA201C适用于吸附和解吸。

The factors and process conditions on purification and preparation of geniposidic acid from alkaline hydrolyzate of exhausted solution of gardenia yellow by macroporous resin were studied.The optimum technology of the preparation of GPA was found according to the decolorization and adsorption- desorption performance of GPA by different resins.The results showed that DA201 weak polar resins had the best decolorization performance and poor absorption of the GPA; DA201 C non- polar resin had higer adsorption rate and desorption rate,reaching88.7% and 98%,respectively.When the amount of resin was 1 g /25 m L 10 mg / m L of GPA crude liquid,p H 4.0,25 ℃,120 r / min,decoloration time 6 h,the decolorization rate reached 85.9%,GPA retention rate reached 92.3%.The optimum conditions for DA201 C resin adsorption of GPA were as follows： destaining solution concentration10 mg / m L,p H 3.0,adsorption velocity 1 BV / h,sample volume 7.2 BV.After eluting with 25% ethanol and drying the eluent,a purity of GPA of 95.1% and a recovery rate of 86.2% were obtained. It showed that DA201 resin was suitable for decolorization and DA201 C resin was suitable for adsorption- desorption of GPA on purification and preparation.