白术中白术内酯Ⅰ,Ⅱ,Ⅲ提取工艺优选

Optimization of Extraction Process of Atractylenolide I,Ⅱ,Ⅲ from Atractylodis Macrocephalae Rhizoma

目的：优选白术中3种内酯类成分的提取工艺。方法：采用HPLC测定白术内酯Ⅰ,Ⅱ,Ⅲ含量,流动相乙腈（A）-水（B）梯度洗脱（0~16 min,60%~76%A;16~18 min,76%~100%A;18~30 min,100%A）,双波长检测220 nm（白术内酯Ⅰ,Ⅲ）和276 nm（白术内酯Ⅱ）。以白术内酯Ⅰ,Ⅱ,Ⅲ提取率为指标,通过单因素试验筛选提取方式,利用正交试验考察乙醇体积分数、溶剂用量、提取时间及提取次数对白术提取工艺的影响。结果：最佳提取方式为乙醇温浸法,最佳工艺条件为加6,4,4倍量90%乙醇于40℃温浸提取3次,提取时间依次为1.5,1.0,1.0 h。白术内酯Ⅰ,Ⅱ,Ⅲ的提取率分别为92.62%,92.39%,93.06%。结论：优选的提取工艺稳定可行,白术中3种内酯类成分的提取率高。

Objective： To optimize extraction technology of atractylenolide Ⅰ,Ⅱ,Ⅲ from Atractylodis Macrocephalae Rhizoma. Method： HPLC was adopted to determine contents of atractylenolide Ⅰ,Ⅱ,Ⅲ with mobile phase of acetonitrile （A） -water （B） for gradient elution （0-16 min, 60% -76% A; 16-18 min, 76% - 100% A; 18-30 min, 100% A） and dual-wavelength detection of 220 nm for atractylenolide I, 11 and 276 nm for atractylenolide II . Taking extracting rates of atractylenolide Ⅰ,Ⅱ,Ⅲ as indexs, extraction method was screened by single factor test, orthogonal test was adopted to optimize extraction process with extracting time, extracting times, ethanol concentration and amount as factors. Result： Alcohol warm infusion method was selected, optimum technological conditions for extracting thrice by adding 6, 4, 4 times the amount of 90% ethanol at 40 ℃ ,extracting time was 1.5, 1.0, 1.0 h in turn. Extracting rates of atractylenolide Ⅰ,Ⅱ,Ⅲ were 92.62% , 92.39% , 93.06% , respectively. Conclusion： This optimized extraction process is stable and feasible with high extraction efficiency of atractylenolide Ⅰ,Ⅱ,Ⅲ in Atractylodis Macrocephalae Rhizoma.