金錢草中總黃酮提取工藝的比較研究

摘    要
金錢草系報(bào)春花科珍珠菜屬植物過(guò)路黃(Lysimachia christinae Hance)的新鮮或干燥全草，主產(chǎn)于四川、浙江等地。金錢草中主要藥效成分為黃酮類化合物，據(jù)有關(guān)文獻(xiàn)報(bào)導(dǎo)，其具有促進(jìn)膽汁分泌和排泄、利尿排石等作用。本文主要研究?jī)?nèi)容和結(jié)果如下：
以金錢草總黃酮含量為指標(biāo)，采用正交試驗(yàn)設(shè)計(jì)優(yōu)選乙醇回流提取法提取金錢草總黃酮的最佳工藝條件為：80%乙醇20倍量，回流提取時(shí)間2.0h，提取次數(shù)為2次。與熱水提取法相比，乙醇回流提取法具有更高的提取效率。
本實(shí)驗(yàn)取用D101型大孔樹脂精制金錢草總黃酮，繼而通過(guò)實(shí)驗(yàn)確定其最佳純化工藝：上樣濃度為0.2mg/mL，6倍量洗滌用水，吸附效果最優(yōu)；以50%乙醇溶液洗脫，洗脫率達(dá)到最高。結(jié)果表明，其純化效果優(yōu)于醇沉法。
本文所建立的金錢草總黃酮提取、純化工藝路線簡(jiǎn)單、高效，易于推廣，為工業(yè)化提取和純化金錢草總黃酮奠定了基礎(chǔ)。

關(guān)鍵詞  金錢草；總黃酮；提?。患兓?；大孔樹脂

Comparison of Extraction Technology of Total Flavonoids from Christina Loosestrife Herb
Abstract
Christina Loosestrife Herb has been long used as a Chinese traditional medicine，which is from flesh or dry plant of Lysimachia christinae Hance，family Primulaceae，This medicinal plant is mainly produced in Sichuan and Zhejiang Province. Flavonoids are the main active ingredients of Christina Loosestrife Herb. It is reported that the total flavonoids in this plant could promote biliation, egestion, urinate and remove urinary calculus. The main contents and conclusions are provided as follows:
The contents of total flavonoids from Christina Loosestrife Herb being served as index, in this topic, ethanol refluxing extraction were selected by orthogonal test. The results were shown that the optimal condition for procedure was extracting 2 h, 4 times with 20 folds of 80% ethanol. Compared with traditional hot water extraction, ethanol refluxing extraction has higher extraction efficiency.
 D101 macro porous resin was used , and the optimal purification conditions was obtained with 0.2mg/mL of total flavonoids concentration、6 folds of water and 50% ethanol as eluting agent. The results were shown that the purification effect was better than the method of ethanol precipitation.
Being simple, efficient and operable, the extraction and purification technology proposed in this research can be used to establish the foundation for extracting and purifying total flavonoids from Christina Loosestrife Herb on industrial scale.
Key words:  Christina Loosestrife Herb; total flavonoids; extraction; purification; macro porous resin
目  錄
摘    要 I
Abstract II
第1章 緒  論 1
1.1 課題背景 1
1.2 金錢草的研究概況 1
1.2.1 金錢草中化學(xué)成分的研究概況 2
1.2.2 金錢草的藥理作用 3
1.2.3 金錢草的臨床應(yīng)用 3
1.2.4 金錢草的不良反應(yīng) 3
1.2.5 本節(jié)小結(jié) 4
1.3 黃酮類化合物的研究現(xiàn)狀 4
1.3.1 黃酮類化合物的提取工藝研究 4
1.3.2 黃酮類化合物的純化工藝研究 6
1.4 本課題研究的內(nèi)容 7
第2章 金錢草中總黃酮提取工藝的比較研究 8
2.1 實(shí)驗(yàn)材料 8
2.1.1 儀器 8
2.1.2 藥材與試劑 8
2.2 方法與結(jié)果 8
2.2.1 標(biāo)準(zhǔn)對(duì)照品溶液的制備 8
2.2.2 供試品溶液的制備 9
2.2.3 顯色方法 9
2.2.4 蘆丁標(biāo)準(zhǔn)品最大波長(zhǎng)掃描 9
2.2.5 標(biāo)準(zhǔn)曲線的繪制 9
2.3 方法學(xué)考察 10
2.3.1 精密度試驗(yàn) 10
2.3.2 顯色穩(wěn)定性考察 10
2.3.3 重現(xiàn)性考察 11
2.3.4 加樣回收率試驗(yàn) 11
2.4 乙醇回流提取金錢草中總黃酮 11
2.4.1 乙醇回流提取方法的單因素考察 11
2.4.2 正交試驗(yàn) 14
2.4.3 正交試驗(yàn)表的選擇 14
2.5 熱水回流提取金錢草中總黃酮 15
2.6 浸膏得率的測(cè)定 15
2.7 兩種提取方法的提取效果比較 15
2.8 討論 15
2.9 本章小結(jié) 16
第3章 金錢草中總黃酮純化工藝的比較研究 17
3.1 實(shí)驗(yàn)材料 17
3.1.1 實(shí)驗(yàn)儀器 17
3.1.2 藥材與試劑 17
3.2 D101型大孔樹脂分離純化金錢草總黃酮 17
3.2.1 大孔樹脂的預(yù)處理及含水率的測(cè)定 17
3.2.2 大孔樹脂的裝柱 18
3.2.3 總黃酮粗提液的制備 18
3.2.4 樹脂的靜態(tài)吸附與解吸 18
3.2.5 D101型大孔吸附樹脂分離純化金錢草總黃酮工藝考察 18
3.2.6 D101型大孔吸附樹脂吸附-洗脫過(guò)程動(dòng)力學(xué)初探 20
3.2.7 大孔樹脂的再生 21
3.3 傳統(tǒng)有機(jī)溶劑純化 21
3.4 兩種純化方法的純化效果比較 21
3.5 討論 22
3.6 本章小結(jié) 22
結(jié)  論 23
1 金錢草中總黃酮的提取 23
2 金錢草中總黃酮的純化 23
致  謝 24
參考文獻(xiàn) 25
附錄 A 27
附錄 B 32