响应面法优化茵陈总黄酮提取工艺及成分结构的初步表征

本文优化了茵陈总黄酮的超声辅助提取工艺并对其成分结构表征进行了研究。在考察提取时间、提取温度、乙醇浓度、液料比对茵陈总黄酮得率影响的基础上,采用Box-Behnken响应面法对提取工艺进行优化,模拟得到二次多项式回归方程的预测模型。采用红外光谱(FT-IR)及液相色谱-质谱联用技术(LC-MS)鉴定了NKA-9树脂纯化后的茵陈黄酮类化合物。结果显示:响应面法优化得到茵陈总黄酮提取的最优工艺为提取温度61 ℃、乙醇浓度48%、液料比30:1 (mL/g),在此条件下,总黄酮得率可达24.89 mg/g。通过对比茵陈提取纯化物与芦丁标准品的FT-IR谱图,表明茵陈提取纯化物中含有C=C、羟基、酚羟基等多种特征官能团的振动吸收峰,是黄酮类化合物的典型结构,并可能含有芦丁单体。通过LC-MS分析茵陈黄酮提取物组成时,通过对比m/z值、保留时间,可推断提取物中含芦丁、金丝桃苷、异槲皮苷、异鼠李素-3-O-葡萄糖苷和香叶木苷等成分。响应面法建立的回归数据模型优化得到的茵陈总黄酮提取工艺实际有效,同时发现提取物中可能含有芦丁、金丝桃苷、异槲皮苷、异鼠李素-3-O-葡萄糖苷和香叶木苷等成分,以期为茵陈提取物的进一步研究提供参考。

Optimization of Extraction Technology by Response Surface Methodology and Preliminary Structural Characterization of the Composition in Flavonoids from Artemisia capillaris

The ultrasound-assisted extraction technology of the flavonoids from Artemisia capillaris was optimized and its structural characterization of the composition were studied in this paper. On the basis of investigating the effect of extraction time,extraction temperature,ethanol concentration and liquid-to-material ratio on the yield of the flavonoids from Artemisia capillaris,the Box-Behnken response surface method was used to optimize the extraction process,and the prediction model of two polynomial regression equations was simulated. The compounds in extract purified by NKA-9 resin were identified by FT-IR and LC-MS. As a result,the optimal extraction process was as follows:extraction temperature of 61 ℃,ethanol concentration of 48%,liquid-to-material ratio of 30:1 (mL:g). Under these conditions,the total flavonoids content was 24.89 mg/g. By comparing the FT-IR spectra of the purified extracts of Artemisia capillaris and the standard rutin,it showed that vibrational absorption peaks of C=C,hydroxyl group,phenolic hydroxyl group and other characteristic functional groups were found in the purified extracts of Artemisia capillaris,which indicated that the extracts had the typical structure of flavonoids and the existence of rutin monomers. LC-MS was used to analyze the constituents of flavonoids in the extract. It was inferred that the extract contained rutin,hyperin,isoquercetin,isorhamnetin-3-O-glucoside and diosmin by comparing m/z value and retention time. The optimal extraction process of total flavonoids from Artemisia capillaris which were established by the regression data model of response surface methodology was practical and effective. It was also found that the extracts might contain rutin,hyperin,isoquercetin,isorhamnetin-3-O-glucoside and diosmin,which can provide reference for the further study of the extract of Artemisia capillaris.