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GC-MS和紫外光譜法分析中國蜂膠乙醇提取物

發(fā)布時(shí)間:2018-05-06 08:19

  本文選題:蜂膠 + 醇提物; 參考:《南昌大學(xué)》2017年碩士論文


【摘要】:為了進(jìn)一步研究中國蜂膠的化學(xué)組成,探索不同氣候帶和顏色蜂膠間的差異,同時(shí)獲得用于分區(qū)的特征化合物。本研究采用氣相色譜質(zhì)譜聯(lián)用(Gas chromatography-mass spectrometry,GC-MS)結(jié)合硅烷化衍生對采自中國22個(gè)省的37個(gè)蜂膠和1個(gè)樹膠的乙醇提取物進(jìn)行成分鑒定,并進(jìn)行多變量分析。另外為實(shí)現(xiàn)對蜂膠進(jìn)行簡便、快捷地初步品質(zhì)檢測,對37個(gè)中國蜂膠的醇提物(Ethanol extract of propolis,EEP)進(jìn)行紫外光譜(Ultraviolet spectrum,UV)掃描,獲得EEP的UV掃描數(shù)據(jù),并進(jìn)行多變量分析,同時(shí)測定EEP的總酚、總黃酮含量、特定吸收率和清除DPPH自由基活性,初步建立回歸模型。研究結(jié)果如下:1.GC-MS結(jié)合硅烷化衍生對37個(gè)蜂膠和1個(gè)樹膠的乙醇提取物進(jìn)行成分鑒定,結(jié)果顯示,37個(gè)EEP共鑒定出124種化合物,包括25個(gè)多酚類化合物,8個(gè)萜類化合物,40個(gè)糖類及其衍生物,且主要是單糖,7個(gè)脂肪酸及其酯類、7個(gè)醇類、7個(gè)酸類、11個(gè)酮類、2個(gè)醚類、9個(gè)甾體類化合物,此外還鑒定出8個(gè)其他類別化合物。其中主要成分為苯甲酸(0.13%~0.48%)、3,4-二甲氧基肉桂酸(0.13%~1.28%)、阿魏酸(0.28~4.02%)、咖啡酸(0.18%~7.14%)和油酸(0.06%~7.56%),以咖啡酸的出現(xiàn)頻率最高,在除了FJ-1、HN-3和HN-4的34個(gè)蜂膠樣品中檢測到。本研究還鑒定出Muco-肌醇、2-氨基-3-羥基苯甲酸甲酯、β-木栓醇、1,1-二-C-辛基,D-葡萄糖醇、羥基錐栗烯酮等40種化合物,均未在前期蜂膠研究中發(fā)現(xiàn)。同時(shí)檢測到咖啡酸、3,4-二甲氧基肉桂酸、對香豆酸、阿魏酸等典型的楊樹型蜂膠化合物,進(jìn)一步證明了中國蜂膠為楊樹型蜂膠。此外在兩個(gè)山東蜂膠樣品中鑒定出白樺脂醇,是樺樹皮的主要成分,說明樺樹可能是其膠源植物之一。主成分分析(Principal component analysis,PCA)結(jié)果表明,黃綠色和黃色蜂膠化學(xué)成分相似,并與黑色蜂膠有較大差異,熱帶蜂膠的糖類化合物含量較高,與其他氣候帶蜂膠差異顯著。線性判別分析(Linear discriminant analysis,LDA)建立判別函數(shù)模型可有效區(qū)分不同顏色蜂膠,雙氫酒石酸、白樺脂醇、α-古蕓烯等19種成分在不同顏色蜂膠中含量差異較大。按氣候帶分類變量,建立判別函數(shù)模型,可有效區(qū)分熱帶蜂膠,其中α-古蕓烯、D-阿拉伯糖、D-果糖等10種化合物在不同氣候帶蜂膠中含量差異較大。2.對37個(gè)中國EEP進(jìn)行UV掃描,并對UV掃描數(shù)據(jù)進(jìn)行PCA和LDA分析,并測定EEP的總酚、總黃酮含量、特定吸收率和清除DPPH自由基活性。結(jié)果顯示,UV掃描數(shù)據(jù)的PCA提取了三個(gè)主成分,累計(jì)貢獻(xiàn)為82.6%,黑色蜂膠與其他顏色蜂膠完全分離;UV掃描積分?jǐn)?shù)據(jù)的PCA分析提取了三個(gè)主成分,累計(jì)貢獻(xiàn)率為92.8%,可將不同品質(zhì)的蜂膠進(jìn)行一定區(qū)分;LDA對蜂膠樣品的分類正確率為97.297%,交叉驗(yàn)證分析成功率為91.891%,該模型可對不同顏色蜂膠進(jìn)行有效區(qū)分,可見多變量分析可有效區(qū)分不同顏色的蜂膠,由于不同顏色蜂膠存在品質(zhì)差異,因此,UV結(jié)合多變量分析可將不同品質(zhì)的蜂膠進(jìn)行區(qū)分。同時(shí),初步建立了總酚、總黃酮含量和清除DPPH自由基活性的多元線性回歸模型。通過對EEP的成分分析,發(fā)現(xiàn)檢測方法對蜂膠成分的鑒定有很大影響,硅烷化衍生結(jié)合GC-MS分析對蜂膠新成分的發(fā)現(xiàn)具有積極作用,結(jié)合多變量分析對研究蜂膠影響因素和化學(xué)組成的關(guān)系具有重要意義。另外UV結(jié)合多變量分析可將不同品質(zhì)的蜂膠進(jìn)行區(qū)分,為蜂膠品質(zhì)的初步鑒定提供了研究思路。
[Abstract]:In order to further study the chemical composition of Chinese propolis, explore the differences between different climatic zones and color propolis, and obtain the characteristic compounds used for zoning. This study uses gas chromatography mass spectrometry (Gas chromatography-mass spectrometry, GC-MS) and silanizing derivatization for 37 propolis and 1 gum from 22 provinces of China The ethanol extracts were identified and analyzed by multivariable. In addition, the preliminary quality detection of propolis was made, the Ethanol extract of propolis (EEP) of 37 Chinese propolis (Ultraviolet spectrum, UV) was scanned by Ultraviolet spectrum, UV, and the EEP UV scanning data were obtained, and the multivariable analysis was carried out. The total phenol, total flavone content, specific absorption rate and DPPH radical scavenging activity of EEP were determined. The results were as follows: 1.GC-MS combined with silanylation was used to identify the ethanol extracts of 37 propolis and 1 gum. The results showed that 124 compounds, including 25 polyphenols, 8, were identified by 37 EEP. Terpenoids, 40 carbohydrates and their derivatives, and mainly monosaccharides, 7 fatty acids and their esters, 7 alcohols, 7 acids, 11 ketones, 2 ethers and 9 steroid compounds. In addition, 8 other types of compounds are identified. The main components are benzoic acid (0.13%~0.48%), 3,4- two methoxy cinnamic acid (0.13%~1.28%) and ferulic acid (0.28~4). .02%), caffeic acid (0.18%~7.14%) and oleic acid (0.06%~7.56%) have the highest frequency of occurrence of caffeic acid in 34 propolis samples, except FJ-1, HN-3 and HN-4. This study also identified 40 kinds of compounds such as Muco- inositol, 2- amino -3- hydroxybenzoate, beta cork alcohol, 1,1- two -C- octyl, D- glucosol, and hydroxy chestnut, and so on. In the propolis study, it was found that caffeic acid, 3,4- two methoxy cinnamic acid, and typical poplar type propolis compounds, such as coumaric acid and ferulic acid, further proved that Chinese propolis was poplar propolis. In addition, betulin was identified in two Shandong propolis samples, which is the main component of birch bark, indicating that birch may be its Principal component analysis (PCA) results show that the chemical composition of yellow green and yellow propolis is similar, and has great difference from black propolis. The sugar content of tropical propolis is higher, and the difference is significant with other climatological propolis. Linear discriminant analysis (Linear discriminant analysis, LDA) has been established. The difference function model can effectively distinguish different color propolis, dihydrotartaric acid, betulinol, alpha palaeolene and other 19 components in different color propolis. According to the climatic zone, the discriminant function model can be established to distinguish the tropical propolis effectively. Among them, 10 compounds, such as alpha palaeolene, D- Arabia sugar and D- fructose, are in different climate. 37 Chinese EEP were scanned by.2. with high content in propolis, and PCA and LDA analysis of UV scanning data were carried out. The total phenol, total flavonoids content, specific absorption rate and DPPH free radical activity were measured for the UV scanning data. The results showed that PCA of UV scanning data was extracted with three main components, and the cumulative contribution was 82.6%, black propolis and other color bees. Three main components were extracted by PCA analysis of UV scan integral data. The cumulative contribution rate was 92.8%, and different qualities of propolis could be distinguished. The classification accuracy of LDA to propolis samples was 97.297%, and the success rate of cross validation analysis was 91.891%. The model could distinguish the different color propolis effectively, and the multivariable component could be seen. In order to distinguish different colors of propolis effectively, because of the quality difference in different color propolis, UV combined with multivariate analysis can distinguish different qualities of propolis. At the same time, the multiple linear regression model of total phenol, total flavone content and DPPH free radical scavenging activity was established. The detection method was found through the analysis of the components of EEP. It has a great influence on the identification of the composition of propolis. Silane derivatization and GC-MS analysis have a positive effect on the discovery of new propolis. Combined with multivariate analysis, it is of great significance to study the relationship between the influence factors and chemical composition of propolis. In addition, UV can be used to distinguish the different quality propolis and the quality of propolis by the combination of multivariate analysis. Step identification provides research ideas.

【學(xué)位授予單位】:南昌大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:O657.63;S896.6

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