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刺玫果提取物化學(xué)成分分離及黃酮苷元的制備

發(fā)布時(shí)間:2018-04-19 23:17

  本文選題:刺玫果 + 黃酮苷元 ; 參考:《吉林化工學(xué)院》2017年碩士論文


【摘要】:刺玫果為野生山刺玫的成熟果實(shí),分布在東北、內(nèi)蒙、山西等地。目前廣泛地應(yīng)用在食品添加劑、功能性飲料、保健食品及藥品等領(lǐng)域。刺玫果中活性物質(zhì)豐富,有黃酮、維生素、皂苷、多糖、三萜類(lèi)等多種化學(xué)成分。藥理學(xué)研究表明,刺玫果具有顯著的抗氧化、抗衰老、促消化和抗輻射作用。本文對(duì)刺玫果黃酮苷元制備、黃酮苷元含量測(cè)定、提取物成分分離等方面進(jìn)行了探索、研究,進(jìn)而促進(jìn)資源豐富、活性廣泛的刺玫進(jìn)一步開(kāi)發(fā)利用。本文首先建立了刺玫果提取物中槲皮素、山奈酚含量的高效液相色譜測(cè)定法,并進(jìn)行了方法學(xué)的考察;其次,在單因素考察的基礎(chǔ)上,利用響應(yīng)面法對(duì)纖維素酶酶解制備黃酮苷元的工藝條件進(jìn)行了優(yōu)化;最后,采用半制備液相、柱層析法、重結(jié)晶法等進(jìn)行刺玫果提取物化學(xué)成分的分離,采用薄層色譜法及高效液相色譜法結(jié)合法對(duì)分離得到的成分進(jìn)行了結(jié)構(gòu)確證。確立了高效液相色譜同時(shí)測(cè)定刺玫果提取物中黃酮苷元--槲皮素、山奈酚含量的分析方法。研究結(jié)果表明:槲皮素在0.0080~0.6000μg的范圍內(nèi)時(shí),其峰面積與進(jìn)樣量線性關(guān)系良好(r=0.9997);山奈酚在0.0025~0.1872μg的范圍內(nèi)時(shí),其峰面積與進(jìn)樣量線性關(guān)系良好(r=0.9995)。槲皮素的平均加樣回收率為103.92%(RSD=0.29%,n=6);山奈酚的平均加樣回收率為95.90%(RSD=0.73%,n=6)。建立的高效液相色譜法操作簡(jiǎn)便、重現(xiàn)性好、結(jié)果準(zhǔn)確,可用于刺玫果黃酮苷元的質(zhì)量控制。以刺玫果提取物為原材料,以酶解后槲皮素峰面積為考察指標(biāo),在單因素考察的基礎(chǔ)上,采用響應(yīng)面法優(yōu)化了酶解法制備刺玫果黃酮苷元的工藝條件。結(jié)果表明,當(dāng)酶解溫度為60.2℃、酶解時(shí)間為2.1 h、酶解pH值為3.2、酶用量為20.0mg/g、料液比為1:150(g:mL)時(shí),刺玫果黃酮苷元的含量最高。采用生物酶解技術(shù)制備黃酮苷元,不但降低了反應(yīng)溫度,還提高了黃酮苷元的得率,具有較大的開(kāi)發(fā)價(jià)值。采用半制備液相、柱層析、重結(jié)晶法從刺玫果提取物中分離得到四種化合物,通過(guò)薄層色譜法及高效液相色譜法對(duì)分離成分進(jìn)行結(jié)構(gòu)確證,四種化合物分別為蘆丁、金絲桃苷、槲皮素、山奈酚,為刺玫果提取物的綜合利用提供了分子學(xué)依據(jù)。
[Abstract]:Rosa davidiflora is the mature fruit of wild Rosa davidiana, distributed in Northeast, Inner Mongolia, Shanxi and other places. At present, it is widely used in food additive, functional beverage, health food and medicine. Rosa davidifolia fruit is rich in active substances, including flavonoids, vitamins, saponins, polysaccharides, triterpenoids and other chemical components. Pharmacological studies showed that Rosa davidifolia had significant antioxidant, anti-aging, digestive and radiation effects. In this paper, the preparation of flavone glycosides, the determination of flavonoid glycosides and the separation of extracts from Rosa davidifolia were studied, so as to promote the further development and utilization of Rosa davurica, which is rich in resources and wide in activity. In this paper, a HPLC method for the determination of quercetin and kaempferol in the extract of Rosa davidifolia L. was established, and the methodology was investigated; secondly, on the basis of single factor investigation, the content of quercetin and kaempferol was determined by HPLC. The reaction surface method was used to optimize the process conditions for the preparation of flavonoid glycosides by enzymatic hydrolysis of cellulase. Finally, the chemical constituents of extracts of Rosa davidiflora were separated by semi-prepared liquid phase, column chromatography and recrystallization. The structure of the isolated components was confirmed by TLC and HPLC. A high performance liquid chromatography (HPLC) method was established for the simultaneous determination of flavonoid glycosides quercetin and kaempferol in the extracts of Rosa davurica. The results show that when quercetin is in the range of 0.0080 ~ 0.6000 渭 g, the linear relationship between peak area and sample amount is good, and the peak area of kaempferol in the range of 0.0025 ~ 0.1872 渭 g has a good linear relationship with the sample quantity. The average recoveries of quercetin and kaempferol were 103.92 and 95.90, respectively. The established HPLC method is simple, reproducible and accurate. It can be used for the quality control of flavonoid glycosides in Rosa davidifolia. The extraction of Rosa davurica was used as the raw material and the peak area of quercetin after enzymatic hydrolysis was used as the index. On the basis of single factor investigation, the reaction surface method was used to optimize the process conditions for the preparation of flavonoid glycosides from Rosa davurica by enzymatic hydrolysis. The results showed that when the hydrolysis temperature was 60.2 鈩,

本文編號(hào):1775177

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