迷迭香黄酮的微波提取及其β-环糊精钾金属有机骨架材料包结物稳定性研究
Microwave-assisted Extraction of Flavonoids from Rosemary and the Stability of Its Potassium-cyclodextrin Metal Organic Frameworks Inclusion Complex
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摘要: 目的:研究迷迭香黄酮的微波提取工艺及其β-环糊精钾金属有机骨架材料包结物(RF-K-CD-MOF)的稳定性。方法:通过单因素实验和响应面法确定微波辅助提取迷迭香黄酮的最佳条件;采用D101大孔树脂纯化迷迭香黄酮,并通过高效液相色谱法(High Performance Liquid Chromatography,HPLC)进行评价;采用溶液包覆法制备RF-K-CD-MOF。结果:最佳提取条件为:乙醇体积分数45%,液料比40:1 (mL:g),微波温度77 ℃,微波功率500 W,提取时间7 min。在此条件下,总黄酮得率为7.88%,黄酮的纯度为30%。纯化后的黄酮纯度由30%提高到70%。黄酮的包结率为87.9%。包埋后迷迭香黄酮的热稳定性及耐酸碱稳定性均有所改善,70 ℃贮存9 d后,总黄酮保存率从20.9%提高到60.6%;对中性环境下稳定性改善作用最显著,总黄酮保存率从41.69%提高到82.58%。结论:响应面法优化迷迭香黄酮提取工艺高效快捷,大孔树脂纯化迷迭香黄酮效果显著,RF-K-CD-MOF的热稳定性及耐酸碱性明显优于迷迭香黄酮提取物。Abstract: Objective:To study the extraction process of rosemary flavonoids and the stability of its potassium-cyclodextrin metal organic frameworks inclusion complex (RF-K-CD-MOF). Methods:The conditions of microwave-assisted extraction of rosemary flavonoids were optimized by single factor experiments and response surface methodology. The extract was purified by D101 macroporous resin,and the purification effect was evaluated by HPLC method. RF-K-CD-MOF was synthesized by solvent method. Results:The optimal extraction conditions were as follows:Ethanol concentration 45%,ratio of liquid to solid 40:1 (mL:g),extraction temperature 77℃,initial microwave power 500 W,and extraction time 7 min. The yield of total flavonoids was 7.88% under these conditions and the purity of flavonoids was 30% in the extract. The purity of flavonoids increased from 30% to 70%. The flavonoids inclusion rate of RF-K-CD-MOF was 87.9%. The heat stability and acid-base resistance of rosemary flavonoids were both improved after embedding,keeping 70℃ for 9 days,the retention of total flavonoids increased from 20.9% to 60.6%. The effect on stability improvement was most significant in neutral environment,the retention of total flavonoids increased from 41.69% to 82.58%. Conclusion:The optimum extraction process of rosemary flavonoids by response surface methodology was convenient and effective,and the effect of macroporous resin for purification of flavonoids was significant. The heat stability and acid-base resistance of RF-K-CD-MOF were better than rosemary flavonoids extracts.