大孔吸附树脂法富集山核桃叶球松素查尔酮工艺的研究

Enrichment of Pinstrobin Chalcone from Leaves of Carya Cathayensis Sarg. by Macroporous Resins

目的:考察10种大孔吸附树脂对山核桃叶球松素查尔酮(pinostrobin chalcone)富集的影响,筛选出富集球松素查尔酮的最佳大孔吸附树脂,并确定富集球松素查尔酮的工艺条件及参数。方法:以球松素查尔酮作为检测指标,进行反相HPLC法进行测定,利用静态吸附方法筛选出最佳大孔吸附树脂为SD200,并利用动态实验优化SD200型大孔吸附树脂富集球松素查尔酮的各种工艺参数。结果:由于SD200型大孔吸附树脂对球松素查尔酮具有较好的吸附力和解吸附力,因此SD200型大孔吸附树脂被选于后续的实验研究。SD200型大孔吸附树脂富集球松素查尔酮的最佳工艺如下:吸附时间为150 min,吸附温度为25℃,样品溶液中球松素查尔酮的浓度为3.58 mg/m L,上样体积为6.5 BV,上样速度为2.0 BV/h,选择70%乙醇溶液进行洗脱,洗脱体积为10.0 BV,洗脱速度为4.0 BV/h。在此条件下,产物中球松素查尔酮的含量从样品溶液中的7.02%提高到26.06%,将近提高了4倍,其回收率为82.81%。结论:SD200型大孔吸附树脂在所确定的工艺条件下,富集球松素查尔酮效果良好,此工艺简单、高效,为球松素查尔酮的大规模制备奠定一定的基础。

Objective： To investigate the influence on enrichment of pinostrobin chalcone with 10 different macroporous resins and to screen the perfect resin and process conditions of enriching pinostrobin chalcone. Method： Using the RP-HPLC method,the content of pinostrobin chalcone in sample solutions was determined. The optimal macroporous resin SD200 was screened by static adsorption tests,and various technological parameters of pinostrobin chalcone enrichment were optimized by dynamic adsorption and desorption tests.Results： The SD200 macroporous resin was used for the following tests because it possessed higher adsorption / desorption capacity and desorption ratio for pinostrobin chalcone. The best process of pinostrobin chalcone enrichment with SD200 macroporous resin was as follows： the adsorption time was 150 min and 25 ℃ was selected as optimal temperature. The proper initial concentration of pinostrobin chalcone in sample solution was 3. 58 mg / m L. The volume and flow rate of sample solution were 6. 5 BV and 2. 0 BV / h in the adsorption process,respectively,and the volume and flow rate of eluting solution were 10 BV ethanol-water solution（ 70： 30,v / v）and 4.0 BV / h in the desorption process,respectively. Through treatment in above perfect conditions,the content of pinostrobin chalcone in product was increased by 4-fold from 7.02% to 26.06%,with a recovery yield of 82.81%.Conclusion：The method established was a promising basis for industry- scale preparation of pinostrobin chalcone from the leaves of Carya cathayensis Sarg.