[關(guān)鍵詞]
[摘要]
目的 對乳香中乳香酸類成分提取純化工藝進行優(yōu)選。方法 采用UPLC-TQ/MS檢測,以乳香中13個乳香酸(3-羰基甘遂-8,24-二烯-21-酸、3α-乙酰甘遂-7,24-二烯-21-酸、3-羥基甘遂烷-8,24-二烯-21-酸、乙酰11α-甲氧基-β-乳香酸、3α-羥基甘燧烷-7,24-二烯-21-酸、11-酮基乳香酸、3-O-乙?;?α-乳香酸、3α-乙酰氧基-羊毛甾-8,24-二烯-21-酸、3β-乙酰氧基-5α-8,24-羊毛甾二烯-21-酸、3-乙?;?11-酮基-β-乳香酸、3-乙?;籽趸仕?8,24-二烯-21-羧酸、α-乳香酸、β-乳香酸)的提取量及浸膏得率為評價指標,通過單因素及響應(yīng)曲面法考察提取方法、提取溶劑、料液比、提取時間及提取次數(shù)對乳香提取工藝的影響;采用堿溶酸沉法純化乳香提取物,并對純化工藝參數(shù)進行單因素和正交試驗考察,確定最佳純化工藝。結(jié)果 以95%乙醇20倍量回流提取4次,每次62 min為最佳提取工藝;以堿液pH為12~13溶解,在0~4℃用酸液pH<2酸沉30 min為最佳純化工藝,乳香酸類成分純度可達73.87%。結(jié)論 此優(yōu)選的提取純化工藝穩(wěn)定可行,適用于乳香有效成分的提取純化,為其物質(zhì)基礎(chǔ)研究提供科學(xué)依據(jù)。
[Key word]
[Abstract]
Objective To optimize the extraction and purification process of the boswellic acids components in the frankincense. Methods The extraction amount and extract yield of 13 boswellic acids (3-oxotirucall-8,24-dien-21-oic acid, 3α-acetoxy-tirucall-7, 24-dien-21-oic acid, 3-hydroxytirucall-8,24-dien-21-oic acid, acetyl 11α-methoxy-β-boswellic acid, 3α-hydroxy tirucall-7,24-dien-21-oic acid, 11-keto-boswellic acid, 3-O-acetyl-α-boswellic acid, 3α-acetyloxylanosta-8,24-dien-21-oic acid, 3β-acetoxy-5α-lanosta-8,24-dien-21-oic acid, 3-acetyl-11-keto-β-boswellic acid, 3-acetyloxy-tirucall-8,24-dien-21-oic acid, α-boswellic acid, β-boswellic acid) in frankincense were detected by UPLC-TQ/MS, the extraction method was investigated by single factor and response surface, the extraction solvent, ratio of solid to liquid, extraction time and extraction times were investigated on the extraction process, and the extract was purified by alkali dissolving acid precipitation method and the purification process parameters were investigated by single factor and orthogonal test to determine the best purification process. Results The optimum condition for the extraction of the frankincense is that twenty times of 95% ethanol for four times reflux extraction and 62 min for each time. Optimum purification process was as following:Dissolve in lye pH 12-13, and the solution was precipitated at 0-4℃ with pH<2 for 30 min. The purity of boswellic acids was 73.87%. Conclusion The optimized extraction and purification process is stable and feasible, which is suitable for the extraction and purification of effective fraction of frankincense and beneficial to give full play to the medicinal value of frankincense and provide scientific basis for material basis research of frankincense.
[中圖分類號]
R283.6
[基金項目]
國家自然科學(xué)基金資助項目(30973885);教育部優(yōu)秀人才計劃項目(NCET-13-0873);江蘇省方劑高技術(shù)研究重點實驗室開放課題資助項目(FJGJS-2015-12)