Page 115 - 精细化工2019年第8期

第 8 期 潘诗哲，等: 响应面法优化荷叶生物碱盐提取工艺及其纯化
mg/g，小于最优工艺中的得率，说明该优化工艺对
提取荷叶生物碱有较好的效果，且该结果高于同等
条件下国标 SN/T 4052—2014 中荷叶碱提取方法的
结果（3.71±0.03 mg/g）和此前一些研究的结果
2.3 D101 大孔树脂纯化荷叶生物碱盐提取物
3 种生物碱的洗脱曲线如图 8 所示（纵坐标百
分比为洗脱出来的量占总量的百分比），乙醇体积分
数为 30%开始有荷叶碱被洗脱出来，故选取体积分
数 30%的乙醇作为除杂液；在乙醇体积分数为 70%
时，得到 100%的 O-去甲基荷叶碱以及 80%左右的
荷叶碱、N-去甲基荷叶碱都被洗脱出来，考虑到乙
醇体积分数过高会洗出更多杂质 [26] ，故选取体积分
数 70%的乙醇作为洗脱液。
图 8 3 种生物碱的洗脱曲线
Fig. 8 Elution curve of three alkaloids
在此基础上，用体积分数 30%乙醇除杂前，先
用氨水将除杂液的 pH 调至 10，防止有生物碱被洗
脱；用体积分数 70%乙醇洗脱前，用盐酸将洗脱液
的 pH 调至 4，强化洗脱效果。用此法纯化后总生物
碱的纯度达到 40.81%。
3 结论
通过单因素实验确定选用盐酸、加热温度 60 ℃、
超声功率 500 W，通过响应面法优化得到荷叶生物
碱盐提取工艺为：盐酸质量分数 0.3%，超声时间
41 min，液固比 27，在此条件下荷叶碱得率为（4.12±
0.05）mg/g，相对误差小于 2%，与预测值误差小于
1%，说明该工艺实际可行。用 D101 大孔树脂纯化
后得到荷叶生物碱盐的纯度达到 40.81%，为今后相
关研究提供参考。
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