节点文献
枣主要活性成分分析及枣蜡提取工艺研究
Analysis of Chemical Bioactive Components and Extraction Technique of Wax in Jujube
【作者】 彭艳芳;
【导师】 刘孟军;
【作者基本信息】 河北农业大学 , 果树学, 2008, 博士
【摘要】 枣(Ziziphus jujuba Mill.)是以营养丰富著称的我国特产优势果树。本文对枣不同品种、器官、不同成熟期果实中的主要活性成分三萜酸、黄酮、皂苷、cAMP(环磷酸腺苷)、膳食纤维进行了研究,并探索了从cAMP糖浆中分离提取枣腊的方法。主要结果如下:1枣总三萜和芦丁测定方法的建立枣总三萜的紫外可见分光光度法经乙酸乙酯或二氯甲烷萃取之后再比色;比色条件:加香草醛-冰醋酸0.4mL,高氯酸1.2mL,70℃水浴20分钟后在580nm处比色。桦木酸、齐墩果酸和熊果酸的HPLC分析法检测波长210nm,流动相为甲醇:水:磷酸=90:10:300ppm,色谱柱:HydersirBDS C18(250mm×4.6mm,5um)。桦木酸、齐墩果酸和熊果酸的测定精密度RSD为4.13%、3.39%和4.28%,加标回收率分别为98.9%(RSD=4.6153)、97.1%(RSD=4.8096)和98.2%(RSD=4.1096)。芦丁的HPLC分析法检测波长210nm,流动相为甲醇:水:磷酸=50:50:500ppm,色谱柱:HydersirBDS C18(250mm×4.6mm,5um)。芦丁的测定精密度RSD为3.39%,加标回收率为100.12%(RSD=3.015 6)。2冬枣和金丝小枣果实成熟过程中主要活性成分的变化总三萜、总皂苷含量均随果实成熟而增加;桦木酸、齐墩果酸和熊果酸在白熟期含量高于全红期,均以桦木酸为主,其次为齐墩果酸、熊果酸。冬枣和金丝小枣的总黄酮、芦丁含量变化均呈倒“V”型。水溶性膳食纤维含量呈缓慢下降趋势;水不溶性膳食纤维和总膳食纤维含量呈缓慢上升趋势。冬枣全红期总三萜、总膳食纤维、水不溶性膳食纤维和cAMP含量均为最高,白熟期总黄酮和水溶性膳食纤维(多糖)含量最高。金丝小枣全红期总三萜含量最高,总黄酮、芦丁、总膳食纤维、水溶性膳食纤维、水不溶性膳食纤维和cAMP含量均为白熟期最高。3枣不同器官活性成分比较枣叶总三萜含量分别是枣果和枣花含量的3.15倍和4.89倍;枣叶桦木酸、齐墩果酸和熊果酸含量分别是枣花和枣果含量的5.38倍和3.58倍,21.71和15.03倍,41.68倍和15.33倍。枣花总皂苷含量最高,其次为枣叶,枣果含量最低;枣花和枣叶总黄酮含量分别是枣果含量的4.01倍和1.17倍。枣花和枣叶芦丁含量分别是枣果含量的29.79倍和18.18倍。枣花水溶性膳食纤维含量分别是枣果和枣叶含量的2.66倍和2.81倍。枣叶总膳食纤维含量分别是枣花和枣果含量的1.85倍和4.20倍。枣叶cAMP含量最高,其次为枣果,枣花未检测出。可见,枣叶和枣花均有很大开发潜力。4枣不同品种主要活性成分的差异对27个枣品种成熟果肉的测定表明:(襄汾)木枣和阜平大枣总三萜含量最高。内黄扁核酸桦木酸含量最高。桐柏大枣、宣城尖枣齐墩果酸含量最高。园铃枣熊果酸含量最高。梨枣、鸡心枣、桐柏大枣总皂苷含量最高。内黄扁核酸总黄酮含量最高。永城长红芦丁含量最高。义乌大枣和内黄扁核酸水溶性膳食纤维含量最高。内黄扁核酸和宣城尖枣水不溶性膳食纤维含量最高。内黄扁核酸总膳食纤维含量最高。湖南鸡蛋枣cAMP含量最高。5枣蜡与环核苷酸糖浆的分离工艺研究枣蜡的最佳提取工艺为:萃取溶剂为乙酸乙酯/乙醇90:10,可溶性固形物含量为70%,萃取次数为2次,萃取倍数为3倍。
【Abstract】 Chinese jujube(Ziziphus jujuba Mill.),a native of China,is famous for its high nutrition content.The contents of the main bioactive components including triterpene acid,flavonoid,saponin,cAMP and edible fiber were compared among cultivars, organs,and different mature stages of fruit.The technology of extraction wax from cAMP syrup was also studied.The main results are as follows:1 Establishment of determination method for total triterpene acid and rutin in Chinese jujubeMethod of the rapid quantification of triterpenoids by ultraviolet spectrometry Color comparation after extracted with AcOEt or dichlorine methanes; The condition for color comparation:adding Citronellal-CH3COOH 0.4 mL,HClO4 1.2 mL,and water bathe at 70℃for 20 minutes,then comparing color at 580 nm.Method of HPLC analysis for betulinic acid,oleanolic acid and ursolic acid Using examination wave-length of 210 nm,mobile phase of methyl alcohol:water: phophoric acid=90:10:0.03%,color composes pillar of HydersirBDS C18(250mm×4.6mm,5um).The variability of measuring betulinic acid,oleanolic acid and ursolic acid is 4.13%,3.39%and 4.28%,respectively;The reclaiming ratio of the three kinds of acisa is 98.9%(RSD=4.6153),97.1%(RSD=4.8096)and 98.2%(RSD=4.1096).Method of HPLC analysis for rutin Using examination wave-length of 360 nm,Mobile phase of methyl alcohol:water:phophoric acid=50:50:0.05%,and color composes pillar of Hydersir BDS C18(250mm×4.6mm,5um).The variability and reclaiming ratio are 3.52%and100.12%(RSD=3.0156),respectively.2 Content variations of bioactive components in the fruits of cultivar ’Dongzao’ and ’Jinsixiaozao’ during fruit maturation The triterpenoid acid and saponin contents kept increasing during fruit rippening.The contents of betulinic acid, oleanolic acid and ursolic acid were higher in white mature stage the in full red stage, of which betulinic acid content kept highest,followed by oleanolic acid,and ursolic acid.The content changes of flavonoid and rutin showed low-high-low type.In ’Dongzao’,the total triterpenoid acid,total fiber,insoluble fiber and cAMP contents reached highest at full-red stage,and the contents of flavonoid and soluble fiber (polysaccharide)reached highest at white-mature stage.In ’Jinsixiaozao’ the contents flavonoid,lutin,total fiber,insoluble fiber and cAMP were highest at white-mature stage,but highest triterpenoid acidcontent appeared at full-red stage.3 Comparation of bioactive component contents among organs of cultivar ’Jinsixiaozao’ The triterpenoid content in leaf is 3.15 4.89 times of that in fruit and flower.The contents of betulinic acid,oleanolic acid and ursolic acid in leaf are 5.38 and 3.58 times,21.71 and 15.03 times,and 41.68 and 15.33 times of those in flower and fruit.The saponin content is highest in flower,followed by leaf and fruit.The contents of flavonoid in flower and leaf are 4.01 and 1.17 times of those in fruit.The rutin contents of flower and leaf are 29.79 and 18.18 times of fruit.The soluble content of flower are 2.66 and 2.81 times of fruit and flower.The total fiber content of leaf are 1.85 and 4.20 times flower and fruit.The cAMP content of leaf is higher than in fruit,and no cAMP was detected in flower.Basing on above mentioned,leaf and flower have very important utilization potential.4 Copareration of bioactive component contents in fruit among cultivars The According to the analysis of 27 cultivars,triterpenoid content is highest in ’Xiangfenmuzao’ and ’Fupingdazao’.The betulinic acid content in ’Neihuangbianhesuan’ is the highest.The oleanolic acid contents are highest in ’Tongbaidazao’ and ’Xuanchengjianzao’.The ursolic acid content is highest in ’Yuanlingzao’.The highest saponin contents were found in ’Lizao’,’Jixinzao’ and ’Tongbaidazao’.The flavonid content is highest in ’Neihuangbianhesuan’.The rutin content of ’Yongchengchanghong’ is the highest.The soluble fiber content of ’Yiwudazao’ and ’Neihuangbianhesuan’ are the the highest.The insoluble fiber content of ’Neihuangbianhesuan’ and ’Xuanchengjianzao’ are the highest.The total fiber content of ’Neihuangbianhesuan’ is the highest.The cAMP content of ’Hunanjidanzao’ is the highest.5 Technique of seperation of wax from cAMP syrup The wax could be well ceperated from cAMP syrup with soluble solid content of 70%by extracting twice with 3 times in volume of extraction solvent(AcOEt:EtOH=90:10).
【Key words】 Chinese jujube; Organ; Cultivar; Bioactive component; Sseperation of wax;