[关键词]
[摘要]
本文以环糊精(α-、β-、或γ-)和淀粉为原料,通过环氧氯丙烷合成水不溶性的环糊精-淀粉树脂(CDP)。比较了三种环糊精-淀粉树脂对落新妇苷的吸附性能,筛选出效果最佳的β-CDP。考察了β-CDP的等温吸附特性,结果表明β-CDP对落新妇苷的吸附量随平衡浓度的升高而增加;吸附过程是一个放热过程,温度升高不利于吸附。4 ℃条件下,落新妇苷平衡浓度为360 μg/mL时,β-CDP的吸附量为49.52 mg/g。该等温吸附可以用Freundlich方程进行拟合,说明β-CDP对落新妇苷的吸附是一个非均匀的多层吸附。比较了不同溶剂对被吸附落新妇苷的解析效果,结果表明60%乙醇为最佳洗脱溶剂,超声处理10 min后解析率为91.97%。将β-CDP用于土茯苓总黄酮的分离纯化,总黄酮得率为2.28%。经HPLC分析产物中落新妇苷含量为51.71%,总黄酮含量为76.63%。
[Key word]
[Abstract]
Three water insoluble cyclodextrin (CD)-starch copolymers (α-, β-, and γ-CDP) were synthesized by using epichlorohydrin as the crosslink reagent. Comparative study of the kinetic adsorptions of α-, β-, and γ-CDP to astilbin showed that β-CDP had the bestabsorption property. Static equilibrium adsorption studies revealed that β-CDP adsorption capacity rose with the increase of equilibrium concentration of astilbin.And its adsorption capacity decreased with the increase of temperature, which revealed that the adsorption was an exothermic process. Under the conditions of 4 ℃ and equilibrium concentration 360 μg/mL, adsorption capacity of β-CDP to astilbin was 49.52 mg/g. The adsorption could quite fit to the Freundlich adsorption isotherm, indicating that it was the nonuniform, multilayer adsorption. About 91.97% of adsorbed astilbin could be recovered by use of 60% ethanol as the elution solvent. The yield of flavonoids was 2.28% when β-CDP was used for separation and purification of flavonoids from Rhizoma Smilacis Glabrae. The contents of astilbin and total flavonoids were 51.71% and 76.63%, respectively, as determined by HPLC.
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[基金项目]
江西省自然科学基金资助项目(20122BAB214005);江西农业大学青年基金资助项目(QN201108)