積雪草苷提取純化工藝研究

制藥工程論文編號:ZY074    論文字數:10700,頁數:28

目  錄
中文摘要 II
英文摘要 III
目錄 IV
1. 緒論 1
 1.1 積雪草苷的理化性質與結構 1
 1.2 積雪草苷的藥理作用 2
 1.3 積雪草苷提取純化工藝的研究 3
 1.4 積雪草苷分析方法的研究 4
2. 實驗部分 5
 2.1 實驗材料和儀器 5
 2.2 積雪草苷的 HPLC方法建立 6
 2.3 正交試驗提取工藝設計 10
 2.4 積雪草苷的分離純化 12
 2.5 薄層色譜法鑒別積雪草苷粗品 14
3. 結果與討論 16
 3.1 積雪草苷提取工藝的結果與討論 16
 3.2 積雪草苷純化工藝路線的結果與討論 19
 3.3 薄層色譜展開劑優化實驗結果與討論 20
4．總結與展望 23
致謝 24
參考文獻 25

摘 要：本文首先建立了HPLC法測定積雪草苷提取物中積雪草苷含量的方法，采用Diamonsil C18柱，乙腈-水（50:50，v/v）為流動相，檢測波長 200nm，結果積雪草苷加標回收率為 100.42℅，RSD為 1.44℅。此方法簡單、準確，適用于積雪草苷提取物的質量控制。然后對積雪草有效成分積雪草苷的提取純化工藝進行了研究。以積雪草苷含量為評價指標，采用 L9(33)正交試驗優選積雪草苷提取工藝，考察了乙醇濃度、料液比、提取時間對積雪草苷含量的影響，最佳工藝為 60℅ 乙醇料液比 1：15回流提取 2h。減壓回收乙醇，得積雪草苷醇提部分。加適量水溶解，以石油醚-乙酸乙酯-正丁醇溶劑系統萃取，正丁醇部分減壓蒸干，溶于少量甲醇，然后滴加丙酮，析出積雪草苷粗品；并與另一條路線：氯仿-正丁醇溶劑系統萃取，正丁醇部分減壓蒸干得積雪草苷粗品進行回收率和含量的比較，得到較優提純工藝。最后采用薄層色譜法對積雪草苷粗品進行檢測，摸索不同展開劑及其配比對積雪草苷粗品的分離情況，以氯仿-甲醇-水（60: 15: 10）及正丁醇-乙酸乙酯-水（4：1：5）的分離效果最好，可為后續進一步的純化提供依據。
關鍵詞：積雪草苷；提取；分離；純化

Abstract: First of all, in this essay established a HPLC method asiaticoside extract content asiaticoside method.Using Diamonsil C18 reserved-phase column, mobile phase as acetonitrile-water （50:50，v/v）elution, detect wavelength at 200nm. The average recovery of asiaticoside is100.42 %, and RSD is 1.44%. This method is simple, accurate and applicable to extract asiaticoside quality control. And then the active ingredients of Centella asiatica asiaticoside the extraction and purification process were studied. Asiaticoside in content for eva luation,To use of L9 (33) orthogonal test asiaticoside preferred extraction process to inspect the ethanol concentration, liquid ratio, extraction time asiaticoside content, the best technology for liquid ethanol 60 ℅ return than 1:15 Extraction of  2h. Decompression ethanol recovery may asiaticoside ethanolic part. Add appropriate amount of water dissolved in petroleum ether - ethyl acetate - n-butanol solvent extraction systems, dry vacuum parts n-butanol, dissolved in a small amount of methanol, and then dropwise acetone, precipitated crude asiaticoside; and another route: chloroform - n-butanol solvent extraction system, vacuum dry n-butanol part of a crude asiaticoside to compare the recovery rate and the content, the better purification process. Finally, the use of thin-layer chromatography of crude asiaticoside test, carried out to explore the different agents and their ratio on asiaticoside separation of crude to chloroform - methanol - water (60: 15: 10) and is butanol - ethyl acetate - water (4:1:5) the best separation for the follow-up to provide a basis for further purification.
Keywords：Asiaticoside; extraction; separation; purification