PMP柱前衍生化HPLC法测定黄秋葵多糖的单糖组成

采用1-苯基-3-甲基-5-吡唑啉酮为柱前衍生化试剂,结合反相高效液相色谱法,建立同时测定黄秋葵多糖中8?种单糖组分的方法。采用InfinityLab Poroahell C18色谱柱为固定相,流动相为磷酸盐缓冲液（0.1?mol/L,pH?6.85）-乙腈（82∶18,V/V）,流速为1.0?mL/min,柱温25?℃,紫外检测器,波长250?nm。各单糖组分的线性范围较宽,相关系数均大于0.999,检出限为0.13～0.45?mg/kg,定量限为0.43～1.49?mg/kg,相对标准偏差小于5%,加标回收率为94.51%～106.44%。方法灵敏度高、准确性好、实用可靠,适用于黄秋葵多糖的单糖组分分析。同时测定从黄秋葵中顺序提取的热水浸提物（hot buffer soluble solution,HBSS）、螯合剂浸提物（chelating agent soluble solution,CHSS）和碱提物（dilute alkaline soluble solution,DASS）的单糖组成,确定其单糖组分的物质的量比。HBSS中,甘露糖∶鼠李糖∶葡萄糖醛酸∶半乳糖醛酸∶葡萄糖∶半乳糖∶阿拉伯糖=0.1∶7.0∶0.4∶5.8∶0.9∶14.6∶1.5;CHSS中,鼠李糖∶半乳糖醛酸∶半乳糖∶阿拉伯糖=4.7∶61.8∶9.6∶5.3;DASS中,甘露糖∶鼠李糖∶半乳糖醛酸∶葡萄糖∶半乳糖∶阿拉伯糖=9.5∶5.4∶1.3∶10.8∶2.4∶7.6。     

响应面试验优化木瓜蛋白酶法脱马齿苋多糖蛋白工艺

为确定木瓜蛋白酶法脱马齿苋多糖蛋白的最佳工艺,以酶液-样液体积比、酶解时间、酶解温度及pH值为影响因素,以马齿苋多糖损失率与蛋白去除率为指标,通过响应面试验优化木瓜蛋白酶法脱马齿苋多糖蛋白的工艺条件。结果表明,木瓜蛋白酶法脱马齿苋多糖蛋白的最佳工艺为酶液-样液体积比0.2∶1、酶解温度60?℃、酶解时间3?h、pH?6,在此条件下蛋白去除率为78.22%,多糖损失率为10.39%。马齿苋粗多糖溶液经分离纯化、高效液相色谱分析,结果表明马齿苋多糖由甘露糖、鼠李糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、半乳糖和阿拉伯糖单糖组成,其组成比例为5.3∶5.9∶1.3∶27.6∶1∶18.8∶14.6。     

A sensitive analytical method for the component monosaccharides of the polysaccharides from a Tibetan herb Potentilla anserine L. by capillary zone electrophoresis with UV detector

A rapid and sensitive method was optimized and validated for the separation and quantification of derivatized monosaccharides in polysaccharide from Potentilla anserine L. using 1-naphthyl-3-methyl-5-pyrazolone (NMP) as precolumn derivatization reagent by capillary zone electrophoresis (CZE). On the basis of the optimum conditions, nine NMP-derivatized monosaccharides achieve baseline resolution within 16 min. The developed method has been successfully applied to analyze component monosaccharides of three Potentilla anserine L. samples, which were obtained by gradational precipitation with 50, 70, and 90% aqueous ethanol, respectively. The polysaccharide precipitated from 50% ethanol solvent was composed of fucose, mannose, xylose, glucuronic acid, glucose, rhamnose, galacturonic acid, galactose, arabinose in molar proportion of 1:1.65:1.99:5.08:7.38:8.14:13.05:27.41:39.02; the corresponding molar proportions for polysaccharide obtained from 70% ethanol solvent were 1:1.64:1.65:4.52:13.96:9.13:26.30:10.52:18.00; fucose and galacturonic acid were not found in the polysaccharide precipitated from 90% ethanol solvent, and mannose, xylose, glucuronic acid, glucose, rhamnose, galactose and arabinose were determined with molar proportion of 1:0.87:1.77:2.78:1.69:2.58:2.49. Quantitative recoveries of the component monosaccharides in the polysaccharide were in the range of 93.3–105.1% and the relative standard deviation (RSD) values fell within 3.4–6.3%, respectively. The results demonstrated that the proposed CZE method was precise and sensitive for the analysis of the composition of polysaccharide.     

蓝靛果多糖功能特性、结构及抗糖基化活性

以蓝靛果果实为原料,采用超声波辅助复合酶法提取,经D4006大孔树脂纯化,制得蓝靛果多糖。并对多糖的功能特性、结构特征和抗糖基化反应活性进行研究。结果表明蓝靛果多糖具有一定的持水性、持油性、乳化性及乳化稳定性;蓝靛果多糖为典型的非牛顿流体,呈现剪切稀释现象,具有作为食品或者生物医药的质地改性剂或增稠剂的潜力;同时蓝靛果多糖热稳定性较好,可作为功能性添加剂应用到食品工业中。气相色谱法测定结果表明,蓝靛果多糖为酸性杂多糖,单糖组成及物质的量比为:半乳糖醛酸-鼠李糖-阿拉伯糖-甘露糖-葡萄糖-半乳糖=2.84∶10.02∶15.47∶1.00∶2.48∶36.12。红外光谱、紫外-可见光谱表明,蓝靛果多糖具有多糖的特征吸收峰,不含核酸、蛋白质和花色苷。刚果红实验、扫描电镜和X射线衍射测定结果显示:蓝靛果多糖不具有三股螺旋结构,呈现无定形片状结构。体外抗糖基化活性测定结果表明蓝靛果多糖对糖基化反应3个阶段产物(Amadori产物、二羰基化合物和糖基化终产物)的形成均表现出良好的抑制作用,质量浓度为0.5 mg/mL时,最大抑制率分别为(35.24±1.44)%、(33.41±1.01)%和(42.62±0.70)%,均高于对照氨基胍。研究结果可为进一步开发利用蓝靛果资源提供一定的理论依据。     

Preliminary studies on the mucilages extracted from Okra fruits,Taro tubers,Jew's mellow leaves and Fenugreek seeds

Okra fruits, Taro tubers, Jew's mellow leaves and Fenugreek seeds are commonly used in Egypt to prepare popular diets with desired slimy consistency.The mucilages were extracted and preliminary studies conducted to characterise them physically. The pH values of a 1% solution of the mucilages varied from 6·9-7·5 for Okra and Taro, 7·1–7·8 for Jew's mellow, and 5·9-6 for Fenugreek, depending upon extraction conditions. The highest viscosity was observed in Okra solutions, followed by Fenugreek, Jew's mellow and Taro mucilages. Okra and Jew's mellow mucilages are acidic polysaccharides which contain higher amounts of ash than the Taro and Fenugreek mucilages which are neutral polysaccharides. All mucilages are associated with protein. Gel chromatography indicated strong interaction of protein with the polysaccharide. The acid hydrolysis of the mucilages followed by paper chromatography revealed that all mucilages contain methyl pentose, glucose, galactose, and fructose, in different proportions. Taro and Fenugreek mucilages are free of rhamnose. All mucilages are devoid of arabinose and mannose except Fenugreek which contained these two sugars.     

莼菜体外胶的分离及其体外功能活性研究

该文以不同物理方法提取的莼菜体外胶为主原料,探讨体外胶本身的物理性能以及生物学特性。结合超声处理研究莼菜体外胶质构性、流变特性、化学物质含量以及抑制酶活性情况,采用GC-MS测定体外胶多糖的单糖组成。结果表明,当超声能量密度为4 800 J/g时,体外胶的分离率最高为(78. 97±3. 83)%。经超声处理后的体外胶的黏度显著降低,在高扫描频率下超声处理会显著增加体外胶的损耗模量(G″),从而增加它的黏性。体外胶含有丰富的总糖(524. 4～552. 8 mg/g)和总多酚(208. 3～228. 5 mg GAE/g),并具有α-葡萄糖苷酶和α-淀粉酶抑制活性。GC-MS分析结果表明,体外胶多糖含有较高含量的半乳糖(41. 79%)和木糖(18. 72%),且含有较少含量的甘露糖(4. 29%),鼠李糖(7. 13%),阿拉伯糖(1. 02%)和葡萄糖(4. 55%)。超声处理不仅会降低体外胶的硬度、弹性、内聚性和黏附性,还有助于体外胶的分离,可以很好地保持体外胶的植物化学物质、抗氧化活性、降血糖活性。     

高效液相色谱法分析地瓜儿多糖的单糖组成

研究分析地瓜儿多糖的单糖组成。采用水提醇沉法提取地瓜儿多糖,用三氟乙酸水解多糖成单糖,单糖产物经衍生化试剂1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化后,利用高效液相色谱法分析单糖的PMP衍生物。结果表明,地瓜儿多糖由甘露糖(Man)、鼠李糖(Rha)、葡萄糖醛酸(GlcUA)、半乳糖醛酸(GalUA)、葡萄糖(Glc)、半乳糖(Gal)、木糖(Xyl)和阿拉伯糖(Ara)8种单糖组成,是一种酸性杂多糖,其中以半乳糖、葡萄糖和半乳糖醛酸为主,为进一步开发利用地瓜儿这一新的野菜资源提供了科学依据。     

鲍鱼内脏多糖的双水相盐析萃取-酶解法提取工艺研究及组成分析

目的建立一种鲍鱼内脏多糖的双水相盐析萃取—酶解法的提取工艺,并对多糖组成进行分析。方法样品经双水相盐析萃取,木瓜蛋白酶酶解醇沉后获得粗多糖。考察鲍鱼内脏干粉的加入量和酶对多糖得率的影响。结果鲍鱼内脏多糖双水相盐析萃取的最适条件为:乙醇30%(V:V)、碳酸钠12%(m:V)和鲍鱼内脏冻干粉加入量7 g/100 mL,酶解最适用酶为木瓜蛋白酶。在此条件下,鲍鱼内脏多糖得率为3.76%。结论经液相色谱分析,该多糖由甘露糖、氨基葡萄糖、鼠李糖、葡萄糖醛酸、半乳糖醛酸、氨基半乳糖、葡萄糖、半乳糖、木糖和岩藻糖组成,其质量比为3.54:2.41:14.75:1.00:1.25:6.79:84.04:7.79:3.38:10.83。     

薇菜多糖的分离纯化及体外抗氧化活性

通过水提醇沉法制备薇菜粗多糖（water-soluble polysaccharide of Osmunda japonica,WOJP）,并用二乙氨乙基（diethylaminoethyl,DEAE）-纤维素层析法对其进行分离纯化,获得2?个多糖组分薇菜中性糖（neutral WOJP,WOJP-N）和薇菜酸性糖（acidic WOJP,WOJP-A）。WOJP-N的分子质量为31.8?kDa,由鼠李糖、半乳糖醛酸、葡萄糖、半乳糖、木糖和阿拉伯糖组成,对应各成分物质的量比为9.1∶5.7∶13.3∶37.6∶5.6∶11.8;WOJP-A的分子质量为15.7?kDa,由鼠李糖、半乳糖醛酸、半乳糖和阿拉伯糖组成,对应各成分物质的量比为7.0∶56.4∶26.1∶5.2。傅里叶变换红外光谱分析结果表明,WOJP-N主要由β-构型的半乳糖组成;WOJP-A主要由吡喃半乳糖醛酸组成,且存在部分酯化修饰。体外抗氧化活性实验结果表明,WOJP的Fe3＋还原能力、1,1-二苯基-2-三硝基苯肼（1,1-diphenyl-2-picrylhydrazyl,DPPH）清除能力和超氧阴离子清除能力与VC相当,具有较好的抗氧化活性,其中WOJP-N和WOJP-A在WOJP发挥抗氧化活性时具有协同作用,两者均是WOJP发挥抗氧化活性的多糖组分。本研究结果可为进一步研究薇菜多糖的构效关系和开发功能性食品提供依据,并为薇菜的应用提供理论参考。     

夏枯草水溶性酸性多糖的分离及活性分析

采用水提醇沉法提取夏枯草多糖,然后经非极性吸附树脂HZ-820 脱色和脱蛋白后,再用DEAE-SepharoseFast Flow 阴离子交换柱层析进行分离得到酸性多糖。化学法和红外光谱证明该酸性多糖中半乳糖醛酸和硫酸根含量较高,间羟基联苯- 硫酸和氯化钡- 明胶比浊法测定其半乳糖醛酸和硫酸根含量分别为(58.85 ± 0.46)% 和(7 ± 0.52)%。紫外、红外光谱分析结果发现,该酸性杂多糖为非糖蛋白,可能含半乳糖醛酸、木糖、葡萄糖、鼠李糖和半乳糖等单糖。抗氧化活性研究表明该酸性多糖具有显著的DPPH 自由基和羟自由基清除活性。     

椰子吸器多糖的结构和体外生物学活性分析

采用水提醇沉法制备了椰子吸器多糖,并初步分析了其单糖组成、分子量大小与分布、红外光谱等结构特征和抗氧化、降糖酶抑制等体外生物学活性。结果表明:吸器多糖是一种酸性杂多糖,中性糖和糖醛酸含量分别为42.33%和21.34%,可能含有吡喃环结构,主要由岩藻糖、鼠李糖、阿拉伯糖、半乳糖、葡萄糖、木糖和半乳糖醛酸7种单糖组成,摩尔比为1.00:4.40:21.27:21.07:51.76:7.06:4.33。分子量分析表明吸器多糖由3个组分构成,其中峰3为主成分,分子质量为1.53×104 g/moL。吸器多糖在6 mg/mL对DPPH和羟自由基的清除率分别为82.49%和85.83%,100 mg/mL时对α-葡萄糖苷酶抑制率达69.91%。研究结果可为椰子吸器在功能性食品或医药等领域的加工利用提供数据支撑。     

石莼多糖的单糖组成成分分析

目的:建立测定分析石莼多糖的单糖组成方法。方法:超声辅助提取石莼多糖,三氟乙酸（TFA）水解多糖,采用薄层色谱法（TLC）和1-苯基-3-甲基-5-吡唑酮（PMP）柱前衍生化高效液相色谱法（HPLC）测定单糖组成。结果:TLC法推断石莼多糖的单糖组成为甘露糖、核糖、鼠李糖、葡萄糖、半乳糖和木糖。PMP-HPLC法表明石莼多糖含有甘露糖、核糖、鼠李糖、葡萄糖、半乳糖和木糖,其摩尔比为:0.08∶0.08∶1.00∶0.97∶0.04∶0.68。结论:TLC法可以对多糖的单糖组成进行定性,但难以进行定量测定。PMP-HPLC法,操作简便,灵敏度高,分离效果好,可用于测定石莼多糖中单糖的组成定性、定量测定。      

梭柄松孢菇子实体中多糖组分及体外抗氧化活性分析

采用热水浸提、85%、95%乙醇分级醇沉制备了两种梭柄松孢菇子实体多糖成分:CVP-85和CVP-95,分析了单糖组成,并测定多糖的体外抗氧化能力。结果表明:CVP-85和CVP-95的得率分别为9.57%±0.23%和5.02%±0.12%;CVP-85中的主要单糖物质为甘露糖、葡萄糖、半乳糖、岩藻糖、葡萄糖醛酸、半乳糖醛酸;CVP-95中的单糖物质有甘露糖、鼠李糖、葡萄糖、半乳糖醛酸。多糖提取物表现出显著的还原能力、DPPH自由基清除能力、羟自由基清除能力、ABTS·清除能力,且在一定浓度范围内,随浓度的增加而显著增强。      

Carbohydrate composition of groundnuts (Arachis hypogea).

The proximate composition of defatted edible groundnut flour, processed and unprocessed, has been determined. The flour contains about 38% total carbohydrates of which oligosaccharides account for 18%, starch 12.5%, hemicelluloses A and B 0.5 and 3.5% respectively and fibre (cellulose) 4.5%. Sucrose 13.90 and 14.55%, raffinose 0.89 and 0.92%, stachyose 1.56 and 1.60%, and verbascose 0.41 and 0.42% represent the oligosaccharide fractions (from 70% alcoholic extract) of unprocessed and processed flour, respectively. In addition the unprocessed flour also contained glucose 0.80% and fructose 0.41 % along with two unidentified spots 0.70%. Hemicellulose A consisted of glucose, arabinose, and xylose (4 : 0.5 : 0.1) whereas hemicellulose B had galacturonic acid, glucose, galactose, arabinose and xylose (1 : 4: 1 : 12 : 6). The fibre fraction on hydrolysis yielded predominantly glucose with only traces of galacturonic acid and rhamnose. The presence of verbascose and xylose in groundnuts has not been previously reported.     

Facile formation of caramel colours using the polysaccharide material that is extracted from the fruit of Azanza garckeana

The mucilage from Azanza garckeana fruit was extracted with water and the extract heated at 130°C in the presence of ammonium salts. When the mucilage, composed of galactose, glucose, arabinose and rhamnose units, was heated, a brown colour was formed. When water was not allowed to evaporate off, the extent of colour formation depended on the initial concentration of the mucilage. The amount of soluble colour that was initially formed decreased as the viscous mass was transformed into a friable insoluble mass. The presence of ammonium salts and pH had only a small effect on the development of colour.     

蓝靛果硒多糖的理化性质、结构表征及红细胞氧化损伤保护活性

以蓝靛果果实多糖为原料,采用微波辅助HNO₃-Na₂SeO₃法制备蓝靛果硒多糖,后经柱色谱分离后得到高含量蓝靛果硒多糖。高含量蓝靛果硒多糖中硒含量为(0.184±0.03) mg/g,重均分子质量为5 88 2 8.3k D a,由半乳糖醛酸、鼠李糖、阿拉伯糖、甘露糖、葡萄糖、半乳糖6种单糖组成,其物质的量比为1∶3.06∶6.18∶0.29∶1.78∶13.01。核磁分析表明高含量硒多糖中存在6种糖苷键,分别为：→3)-β-D-半乳糖(1→、→4)-β-D-甘露糖-(1→、→6)-α-D-葡萄糖-(1→、→4)-α-D-半乳糖醛酸-(1→、→2,4)-α-L-鼠李糖-(1→、α-L-阿拉伯糖-(1→。红细胞氧化损伤保护实验结果表明：同H₂O₂处理红细胞损伤组相比,保护组高含量蓝靛果硒多糖质量浓度为10.0 mg/mL时,H₂O₂诱导的红细胞氧化溶血率降低了32.52%;活性氧水平降低了44.93%;丙二醛含量减少了17.04 nmo...     

Changes in the ethanol-insoluble material of tea leaves (Camellia sinensis L.) during maturation

The ethanol-insoluble material (e.i.m.) of immature and mature tea leaves was fractionated into hot-water-soluble polysaccharides and proteins, ammonium oxalate-soluble pectic acid, hemicelluloses A and B and α-cellulose, by successive extraction with hot water, ammonium oxalate, sodium hypochlorite and cold alkali. The final residue was termed α-cellulose. The hot-water extract and the hot-water-insoluble residue were found to contain appreciable quantities of protein nitrogen. Each fraction was hydrolysed and the mixture of sugars was separated on paper chromatograms and estimated. It appeared that each stage of the extraction procedure removed from the e.i.m. a complex mixture of polysaccharides. The sugars produced on hydrolysis of the arbitrary fractions from immature and mature leaves were qualitatively similar, although there were quantitative differences and were glucose, galactose, xylose, arabinose, rhamnose, galacturonic acid and an unidentified uronic acid. Maturation was mainly accompanied by an increase in the content of lignin, hemicelluloses and α-cellulose.     

桑叶多糖的化学组成及其对胰脂肪酶的抑制作用研究

将复合酶辅助热水提取所得的桑叶粗多糖依次进行脱蛋白和脱色处理后得到桑叶多糖,研究其化学组成和对胰脂肪酶的抑制作用及作用类型。结果表明,桑叶多糖的总糖含量为58.28%,其单糖组成及摩尔比为甘露糖:鼠李糖:葡萄糖:半乳糖:木糖:阿拉伯糖:葡萄糖醛酸:半乳糖醛酸=8.61:23.42:4.23:12.73:1.31:3.06:41.40:123.32。桑叶多糖对胰脂肪酶有一定抑制作用,其半数抑制浓度(IC50)为10.32 mg/mL,抑制作用类型为非竞争性抑制。桑叶多糖有望作为胰脂肪酶抑制剂用于减肥保健食品的加工。     

微波提取对胡萝卜中的多糖基本结构特征及固体形貌的影响

研究微波提取对胡萝卜中的多糖基本结构特征及固体形貌的影响。采用沸水浴、微波两种方式提取胡萝卜中的多糖(分别记为WEP和MEP),通过基本理化性质测定、高效体积排阻色谱(high performance size exclusion chromatography,HPSEC)和单糖组成分析等方法比较了两者的基本结构特征,并采用扫描电子显微镜对两者的固体形貌进行表征。结果显示,WEP和MEP的中性糖、糖醛酸和总酚含量存在差异,两者均由半乳糖醛酸、半乳糖、葡萄糖、阿拉伯糖、鼠李糖组成,但MEP总糖含量更高并含有更多果胶类单糖;WEP和MEP的HPSEC图有一定相似性,但WEP中含有重均分子质量高达7.77×105 D的组分;WEP表现较为聚集的片状结构,而MEP组分则表现较为分散且主要为小片段状态。上述结果表明,两种不同提取方法所得到的多糖具有显著差异。     

薜荔胶主要组成的研究

研究了薜荔胶的主要化学组成。结果表明 ,薜荔胶是以多聚半乳糖醛酸为基本结构的果胶类物质 ,其半乳糖醛酸含量为 76 2 % ,酯化度为 40 8% ,属低酯果胶 ;气相色谱分析结果表明 ,薜荔胶含有鼠李糖、葡萄糖、半乳糖、甘露糖、阿拉伯糖和木糖等中性糖基 ;以粘度法测得薜荔胶的表观相对分子质量为 3 3 5× 10 5。