發(fā)布時(shí)間：2018-03-10 09:03

  本文選題：綠原酸　切入點(diǎn)：高純度　出處：《中國科學(xué)院煙臺(tái)海岸帶研究所》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：綠原酸(CGA)作為一種重要的天然多酚物質(zhì),具有顯著的降血壓、滋肝潤膽、抗菌、預(yù)防腫瘤等多種藥理活性,是許多中成藥的有效成分,近年來在不斷受到人們的重視,并被廣泛應(yīng)用于化妝品、食品、醫(yī)藥等行業(yè)。因此,研究高純度綠原酸的制備工藝技術(shù),對(duì)我國國民經(jīng)濟(jì)和社會(huì)發(fā)展具有重要意義。本論文以杜仲葉粗提物為實(shí)驗(yàn)原料,通過嚴(yán)謹(jǐn)?shù)膶?shí)驗(yàn)設(shè)計(jì),研究出了一條容易操作,穩(wěn)定可靠的高純度綠原酸制備工藝路線,并在此基礎(chǔ)上進(jìn)行了中試放大研究,所得主要研究結(jié)果如下:(1)定量方法的建立以高效液相色譜儀為檢測儀器,建立了定量檢測杜仲葉粗提物中綠原酸的方法,并對(duì)其進(jìn)行方法學(xué)驗(yàn)證。結(jié)果顯示,該HPLC法基線穩(wěn)定,綠原酸與其他成分分離度高,回收率高,因此可以作為杜仲葉提取物中綠原酸的檢測和定量分析方法。(2)大孔樹脂初步分離純化篩選出ADS-21最佳大孔吸附樹脂,并發(fā)現(xiàn)該樹脂在25℃條件時(shí)達(dá)到最大吸附量,同時(shí)滿足Langmuir方程和偽二級(jí)動(dòng)力學(xué)方程。ADS-21樹脂分離純化粗提物中綠原酸的最佳工藝條件為:1)吸附:吸附液pH=2,溫度25℃,上樣流速2 BV/h,上樣濃度3.01 mg/m L,上樣體積8 BV;2)解吸:解吸流速2 BV/h,乙醇濃度及用量為40%乙醇3 BV,50%乙醇10 BV。通過大孔樹脂吸附解吸一次純化后,得到綠原酸粗品的純度由原來的5.01%提高到38.1%,提高了7.62倍,綠原酸回收率為92.8%。(3)樹脂和硅膠除雜精制采用樹脂和硅膠精制綠原酸粗品,通過研究得到X-5樹脂除雜最佳工藝條件:pH≈6,當(dāng)層析柱直徑:高(cm:cm)=3.5:35時(shí),料液比為M:V(g:mL)=1:10;硅膠除雜最佳工藝條件:當(dāng)玻璃層析柱直徑:高(cm:cm)=3.5:35時(shí),料液比為M:V(g:m L)=1:100。解吸濃縮液通過硅膠和X-5型樹脂吸附除雜后,綠原酸的純度由38.1%提高到73.2%,產(chǎn)率65.3%。(4)活性炭脫色精制以活性炭為脫色材料對(duì)綠原酸粗精品進(jìn)行精制,得到最佳脫色工藝條件為:1)吸附:200目以上活性炭,溫度30℃,料液比M:V=2:50(g:mL),時(shí)間1.5 h;2)解吸:溫度50℃,乙醇濃度50%,時(shí)間5 h,解吸量7 BV,解吸三次。通過活性炭脫色精制后,得到純度為93.4%接近無色的綠原酸精品,產(chǎn)率為88.7%。(5)實(shí)驗(yàn)室放大研究實(shí)驗(yàn)室放大研究結(jié)果表明,放大實(shí)驗(yàn)和預(yù)實(shí)驗(yàn)所得綠原酸精品的純度和總得率基本一致,均在92%和60%左右。因此,該工藝技術(shù)路線總體穩(wěn)定,實(shí)用可靠,適用于從杜仲葉粗提物中工業(yè)化制備高純度綠原酸。
[Abstract]:As an important natural polyphenol, Lv Yuan has many pharmacological activities, such as lowering blood pressure, nourishing liver and gallbladder, antibacterial, preventing tumor and so on. It is an effective component of many Chinese patent medicines, and has been paid more and more attention in recent years. It is widely used in cosmetics, food, medicine and other industries. Therefore, it is of great significance to study the preparation technology of high purity Lv Yuan acid for the development of national economy and society in China. In this paper, the crude extract of Eucommia ulmoides leaves is used as experimental material. Based on the rigorous experimental design, a stable and reliable process for the preparation of high purity Lv Yuan acid was developed, and on the basis of this, the pilot scale up study was carried out. The main results are as follows: (1) Establishment of quantitative method for quantitative determination of Lv Yuan acid in crude extract of Eucommia ulmoides leaves with high performance liquid chromatograph (HPLC). The results show that the baseline of this HPLC method is stable. Lv Yuan acid has high separation degree from other components and the recovery rate is high. Therefore, Lv Yuan acid can be used as a method for the detection and quantitative analysis of Lv Yuan acid in Eucommia ulmoides leaves extract. The macroporous resin can be preliminarily separated and purified by macroporous resin, and the best macroporous adsorption resin can be obtained. It was found that the maximum adsorption capacity of the resin was achieved at 25 鈩，

本文編號(hào)：1592647