天麻中总多酚的大孔树脂纯化工艺优化
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篇名: 天麻中总多酚的大孔树脂纯化工艺优化
TITLE:
摘要: 目的:建立天麻中总多酚的含量测定方法,并对其大孔树脂的纯化工艺进行优化。方法:采用福林酚比色法测定天麻中总多酚的含量。以吸附、解吸性能为考察指标,采用静态吸附和解吸试验对4种大孔树脂进行筛选,采用动态吸附和解吸试验对上样液流速、上样液质量浓度、洗脱溶剂体积分数、洗脱流速、洗脱液体积进行考察,从而对其纯化工艺进行优化。结果:没食子酸检测质量浓度的线性范围为4~32 μg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD均小于2%;加样回收率为95.51%~102.94%(RSD=2.54%,n=6)。D301型大孔树脂对天麻中总多酚的静态吸附和解吸能力相对较强;最优纯化工艺为上样液流速2倍柱体积/h,上样液质量浓度4 mg/mL,洗脱溶剂(乙醇)体积分数70%,洗脱流速3 BV/h,洗脱溶剂体积5 BV。按最优纯化工艺优化后的天麻中总多酚含量为0.381 mg/g。结论:所建含量测定方法灵敏度高、稳定性好;优化的纯化工艺稳定、可行。
ABSTRACT: OBJECTIVE: To establish a method for content determination of total polyphenols from Gastrodia elata, and to optimize the purification technology of macroporous resin. METHODS: The content of total polyphenols from G. elata was determined by Folin-ciocaileu colorimetry. Using the absorption and desorption performance as index, 4 kinds of macroporous adsorption resins were selected by static adsorption and desorption tests. The flow rate and mass concentration of the sampling solution, volume fraction of eluent, eluent flow rate and eluent volume were investigated by dynamic adsorption and desorption tests. The purification technology of macroporous resin was optimized. RESULTS: The linear range of gallic acid was 4-32 μg/mL (r=0.999 9). RSDs of precision, stability and repeatability tests were all less than 2%. The recovery rate of the sample was 95.51%-102.94%(RSD=2.54%,n=6). D301 macroporous resin had strong static adsorption and desorption ability from G. elata polyphenols. The optimal purification technology included that the sample solution flow rate 2 BV/h; the sample solution mass concentration 4 mg/mL; the elution solvent 70% ethanol; the elution flow rate was 3 BV/h, and the eluent volume 5 BV. The content of total polyphenols from G. elata optimized by the optimal purification technology was 0.381 mg/g. CONCLUSIONS: Established method is sensitive and stable. The optimized purification technology is stable and feasible.
期刊: 2019年第30卷第14期
作者: 蔺蓓蓓,郑红星,刘祥,周天华,胡红忠,陈琛
AUTHORS: LIN Beibei,ZHENG Hongxing,LIU Xiang,ZHOU Tianhua,HU Hongzhong,CHEN Chen
关键字: 天麻;总多酚;大孔树脂;福林酚比色法;纯化工艺
KEYWORDS: Gastrodia elata; Total polyphenols; Macroporous resin; Folin-ciocaileu colorimetry; Purification technology
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