新疆药桑叶、枝多糖中单糖的组成分析与测定

目的:分析新疆药桑叶、枝多糖中单糖的组成并对其进行测定。方法:采用水提醇沉法提取新疆药桑叶、枝中的多糖,用2mol·L-1H2SO4将多糖水解成单糖,以1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化;采用反相高效液相色谱法测定各单糖。结果:桑叶、桑枝多糖均是由甘露糖、鼠李糖、葡糖醛酸、半乳糖醛酸、葡萄糖、半乳糖、阿拉伯糖等单糖组成。7种单糖在25min内可很好地分离。结论:本方法操作简便、灵敏度高、结果准确,可用于新疆药桑的质量控制。     

威灵仙多糖的分离纯化及其理化性质

目的:对威灵仙多糖进行分离纯化,并进行组成和理化性质分析。方法:威灵仙根经热水提取、DEAE-SepharoseFF柱层析得到威灵仙多糖CCP-Ⅰ、CCP-Ⅱ、CCP-Ⅲ3个组分。CCP-Ⅲ再经Superdex-200柱层析得到威灵仙多糖CCP-Ⅲa、CCP-Ⅲb。通过HPLC和比色等方法对CCP-Ⅲa、CCP-Ⅲb进行分析测定,采用红外、气相色谱、高碘酸氧化等手段对其结构进行初步研究。结果:CCP-Ⅲa为均一组分,其总糖含量、糖醛酸含量分别为92.4%,27.6%,相对分子质量为3.1×105Da,单糖组成及摩尔比为鼠李糖-阿拉伯糖-甘露糖-葡萄糖-半乳糖(4.7∶1.0∶5.6∶26.4∶3.9);CCP-Ⅲb也为均一组分,其总糖含量、糖醛酸含量分别为89.9%,39.5%,相对分子质量为1.5×105Da,单糖组成及摩尔比为鼠李糖-甘露糖-葡萄糖-半乳糖(1.5∶1.0∶25.8∶16.3)。糖苷键主要为β-构型,且均含有1→3、1→6连接键型。结论:CCP-Ⅲa和CCP-Ⅲb是2种均一的酸性杂多糖。     

白蔹多糖PAJM-Ⅰ的分离纯化和结构分析

目的从白蔹中提取分离白蔹多糖,并研究其结构性质。方法经热水提取、乙醇沉淀、Sevag法脱蛋白后得到粗多糖PAJM,进一步用DEAE-Sapharose Fast Flow,Sephadex G-200分离纯化得到PAJM-Ⅰ,对分离到的主要多糖应用高碘酸氧化、高效凝胶渗透色谱(HPGPC),GC,GC-MS,IR等方法进行结构分析。结果提取纯化的白蔹多糖(PAJM-Ⅰ)是均一的多糖,相对分子量为3.25×104,鼠李糖,木糖,甘露糖和半乳糖组成摩尔比为:12.98∶23.52∶45.06∶18.44。分子中1→3,1→2,1→6连接的糖苷键数比为51%∶26%:23%。结论首次从白蔹中分离得到PAJM-Ⅰ均一多糖,且PAJM-Ⅰ含有α-D-葡萄吡喃糖。     

蜜环菌多糖的分离纯化及PMP衍生化HPLC分析

目的:对蜜环菌发酵液进行多糖的提取、分离纯化,得到均一多糖,对其进行单糖组分分析.方法:分离纯化采用分步醇沉和葡聚糖凝胶(Sephadex G-200)色谱法;纯度鉴定及分子量测定采用高效液相色谱法;单糖组成采用1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生HPLC法测定.结果:获得两种均一多糖(AMFP-Ⅰ、AMFP-Ⅱ),峰位分子量分别为 812 939D、596 217D,重均分子量(MW)分别为995 098D、872 640D,分布宽度(Mw/Mn)分别为1.268 93、1.235 20;测定单糖组成为甘露糖、鼠李糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、半乳糖、木糖、阿拉伯糖.结论:两种多糖分子量分布及单糖组成均不同,AMFP-Ⅰ主要由半乳糖醛酸、葡萄糖、半乳糖组成,AMFP-Ⅱ主要由半乳糖醛酸、半乳糖、木糖组成.     

人工培养蛹虫草多糖的分离纯化及其结构的初步研究

目的人工培养蛹虫草多糖类成分的提取与纯化。方法采用SephadexG 10 0柱色谱法进行了分离纯化 ;通过理化常数测定、化学和光谱分析等方法研究了其化学结构特征。结果分离得到CPS 1、CPS 2和CPS 33种多糖 ,其单糖组成分别为 :CPS 1:鼠李糖 木糖 甘露糖 葡萄糖 半乳糖 (1∶6 .4 3∶2 5 .6∶16 .0∶13.8) ;CPS 2 :鼠李糖 葡萄糖 半乳糖 (1∶4 .4 6∶2 .4 3) ;CPS 3为只含葡萄糖的均一多糖。 3种多糖的分子量分别为 2 30 0 0、12 90 0和 5 0 0 0。CPS 1主要含有β糖苷键 ,CPS 2和CPS 3主要含有α糖苷键。 结论CPS 1为一种含有 5种单糖 ,糖苷键为 β构型的多糖 ;CPS 2是一种含有 3种单糖 ,糖苷键为α构型的多糖 ;CPS 3是一种仅含葡萄糖、糖苷键为α构型的多糖     

具有网状内皮系统活性的几种中药多糖的研究

从几种中药的热水提取物中分离到11种多糖,它们能显著增强网状内皮系统(RES)的活力。这些多糖对RES的作用是用改良的ICR-SPF雄性小鼠体内碳廓清试验证明的。用化学和光谱方法阐明了这些免疫活性多糖的结构特征。从防风(Saposknikovia divaricata)根和根茎中分到防风多糖A、B、C(saposknikovans A、B、C)。多糖A的主链为α-1→4-D-聚半乳糖醛酸,侧链为α-1→5-L-阿拉伯糖-β-3,6-分支D-半乳聚糖,多糖C则具有果胶样聚鼠李糖半乳糖醛酸主链和α-3,5-分支-L-阿拉伯聚糖和β-3.4-分支-D-半乳聚糖。从冬葵(Malva verticillata)中分得一中性     

绿藻硫酸多糖UCS2的结构及抗凝血活性研究

目的 对绿藻多糖UCS2的结构特征和抗凝血活性进行研究。方法 通过冷水提取、强阴离子交换色谱和凝胶渗透色谱,从绿藻花石莼中提取分离得到硫酸多糖UCS2;采用高效凝胶渗透色谱（HPGPC）、高效液相色谱、红外光谱和气质联用色谱对多糖UCS2的结构进行表征;通过活化部分凝血活酶时间（APTT）、凝血酶时间、凝血酶原时间对多糖UCS2体外抗凝血活性进行研究。结果 绿藻多糖UCS2分子量为39.55kDa,硫酸根和糖醛酸含量分别为19.74%和18.66%;UCS2主要由鼠李糖组成,含有少量葡糖醛酸和木糖。糖链中含有→3,4)-α-L-Rhap-(1→, →4)-α-L-Rhap-(1→, →4)-β-D-Xylp-(1→和→4)-β-D-GlcAp-(1→,硫酸基位于→4)-α-L-Rhap-(1→的C-3位。多糖UCS2对APTT有显著延长作用,具有较高的抗凝活性。结论 绿藻多糖UCS2是1种抗凝活性的葡萄糖醛酸-木糖-鼠李糖型硫酸多糖。     

柱前衍生化–高效液相色谱法测定蒙古黄芪多糖中单糖的组成

目的测定蒙古黄芪多糖中的单糖组成。方法蒙古黄芪多糖样品用三氟乙酸溶液水解成单糖,用1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化,采用HPLC法于245nm波长处检测各单糖。结果蒙古黄芪多糖由甘露糖、鼠李糖、半乳糖醛酸、葡萄糖、阿拉伯糖组成,物质的量比分别为0.02∶0.05∶0.17∶1∶0.18。结论此方法简单、快速、重复性好,可用于蒙古黄芪多糖中单糖组成分析。     

柱前衍生-高效毛细管电泳法测定刺糖多糖中单糖的组成

目的:分析测定刺糖多糖中单糖的组成。方法:将刺糖多糖水解成单糖,1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化,采用高效毛细管电泳法在245 nm紫外检测分离测定各单糖。结果:刺糖多糖中阿拉伯糖、葡萄糖、鼠李糖、半乳糖、甘露糖、葡萄糖醛酸、半乳糖醛酸的摩尔比为2.80∶38.61∶5.28∶3.76∶1.91∶3.82∶2.45,且刺糖多糖中葡萄糖的含量为35.65%。结论:本法测定刺糖多糖的单糖组分操作简便,灵敏度高,结果准确可靠,可用于刺糖多糖单糖组成测定和质量控制。     

新型糖组成高效液相色谱分析技术的构建及其在水飞蓟多糖质控中的应用

本研究采用1-苯基-3-甲基-5-吡唑啉酮 (PMP) 作为还原醛糖的标记识别分子, 利用高效液相色谱-紫外检测器 (HPLC-UV) 和普通C₁₈色谱柱, 建立了10种常见单糖在13.5 min内的快速HPLC-UV分析鉴别技术, 并成功地用于植物药水飞蓟多糖中单糖的组成分析。结果表明, 醛糖的PMP标记与流动相三乙胺 (TEA) 配比分离调节相结合, 可大幅度调节系列单糖PMP标记物的分离度, 具有很高的分离可控性; 水飞蓟多糖由甘露糖、鼠李糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、木糖、半乳糖及阿拉伯糖8种单糖组成, 其摩尔比为0.66∶0.84∶0.58∶1.0∶1.6∶0.69∶2.7∶4.8; 样品测定回收率为92.4%～104.0%。该方法简单、快速、准确, 可用于水飞蓟多糖的有效质量控制。     

板蓝根多糖A的分离纯化及结构研究

目的:提取分离板蓝根中均一分子量多糖成分,并对其结构进行研究。方法:从板蓝根中提取水溶性粗多糖,经柱色谱分离纯化得到板蓝根多糖A。采用高效凝胶色谱法检测纯度及相对分子量。经UV、IR、NMR和高碘酸氧化、Smith降解法研究各多糖的化学结构。结果:板蓝根多糖A的相对分子量为11700,主要单糖组成为阿拉伯糖和半乳糖,糖苷键构型以α为主,连接方式以1→3键连接为主,并同时存在1→2和(或)1→4的连接方式。结论:板蓝根多糖A的纯度均在96%以上,是一个新化合物。     

Purification and structural analysis of a novel polysaccharide from Rehmannia Radix Praeparata

In this paper, the purification, structure, and antioxidant activity of Rehmannia Radix Praeparata polysaccharide (RRPP) were studied. The RRPP was separated using DEAE-52 cellulose and Sephadex G-100. The RRPP consisted of xylose, glucose, rhamnose, galactose, and mannose in ratios of 10.64:5.58:3.52:1.39:1.0. No protein was detected in the RRPP fraction, and the molecular weight of RRPP was about 1.75 × 10⁶ Da. The basic skeleton information was obtained using periodic acid oxidation—Smith degradation, and RRPP contained 1→, 1 → 2, 1 → 3, 1 → 4, 1 → 2,6, 1 → 4,6 or 1 → 6, 1 → 2,3, 1 → 2,3,4, and other glycosidic bonds. Fourier transform infrared spectroscopy also showed that RRPP has both α- and β-glycosidic bonds. The in vitro antioxidant activity test showed that RRPP could potentialize scavenging effect on ABTS^+· and its scavenging rate was 91.3%.     

A polysaccharide from the stems of Rubus amabilis Focke and its immunological enhancement activity

A water-soluble polysaccharide (named RAP) was newly isolated from the stems of Rubus amabilis. Structural confirmation of the polysaccharide was provided by hydrolysis, periodate oxidation, Smith degradation, and methylation analysis, combined with nuclear magnetic resonance (NMR), capillary electrophoresis (CE), infrared spectroscopy (IR), and gas chromatography-mass spectra (GC-MS). In vitro immunological enhancement activity was characterized using the proliferative activity of spleen lymphocytes and phagocytic activity of peritoneal macrophages in mice. The polysaccharide was mainly composed of xylose, arabinose, glucose, rhamnose, galactose, mannose, glucuronic acid, and galactocuronic acid in the molar ratio of 1.0:6.9:0.8:1.1:6.9:0.3:0.5:3.3, with the average molecular weight of 26.2 kDa. The linkage types of netural monosaccharides were as follows: the arabinose was →2) Ara (1→ and galactose were Gal (1→, →3) Gal (1→, →3,6) Gal (1→, →2,3,6) Gal (1→ and →2,3,6) Gal_f (1→. Xyl (1→, →6) Glc (1→, →2) Glc (1→, →3) Rha (1→, Rha (1→ and Man (1→ were also found in the structure. RAP-B-2 could improve the proliferative activity of spleen T cells and B cells and boost phagocytic activity of peritoneal macrophages at the concentration of 50 μg/ml (p < 0.05, p < 0.01).     

Development and application of a capillary electrophoretic method for the composition analysis of a typical heteropolysaccharide from Codonopsis pilosula NANNF

A simple capillary electrophoretic method based on 1-phenyl-3-methyl-5-pyrazolon (PMP) derivatization has been developed for simultaneous separation and determination of nine aldoses (xylose, arabinose, glucose, rhamnose, fucose, galactose, mannose, glucuronic acid and galacturonic acid). The separation of PMP-labeled monosaccharide derivatives was carried out in uncoated capillary (48.5 cm x 75 microm i.d.) and under the selected optimum conditions of pH 11.0, 200 mM borate buffer at applied voltage 15 kV and capillary temperature 20 degrees C, the nine PMP-monosaccharides could be perfectly separated from each other within 40 min. Furthermore, the developed method was firstly applied to determine the sugar composition in the polysaccharide isolated from Chinese Codonopsis pilosula. The results showed that C. pilosula polysaccharide was a typically acidic heteropolysaccharide and was composed of arabinose, glucose, rhamnose, galactose, mannose, glucuronic acid and galacturonic acid in the molar contents of 48.1, 103.5, 16.1, 48.5, 7.5, 4.2 and 119.1 microM, respectively. The assay results were satisfactory.     

黄芪多糖的研究

从中药黄芪Aslragalus mongholicus Bunge.的水提液中分离得到两种葡聚糖AG-1、AG-2和两种杂多糖AH-1、AH-2。该四种多糖经电泳、凝胶柱层析等证实均为单一组分。AG-1为水溶性,经水解、过碘酸氧化、甲酸生成、Smith降解、乙酰解、红外、C-13核磁共振等确定为α(1→4)(1→6)葡聚糖、α(1→4)与口(1→6)甙键糖基的组成比例约为5:2。AG-2不溶于水,为α(1→4)葡聚糖。AH-1为水溶性酸性多糖,水解后纸层析检出含己糖醛酸(半乳糖醛酸和葡萄糖醛酸)、葡萄糖、鼠李糖、阿拉伯糖,其分子比值为1:0.04:0.02:0.01。AH-2为水溶性、水解后用纸层析和气相层析检出葡萄糖和阿拉伯糖,其分子比值为1:0.15。AG-1、AH-1具有某些免疫促进作用。     

人参果胶的纯化与鉴定

人参果胶经分离、纯化获两种(SA、SB)酸性杂多糖。经醋酸纤维薄膜电泳、玻璃纤维纸电泳分别呈章一色斑。SA的组成以中性糖为主,其中半乳糖、阿拉伯糖、鼠李糖间摩尔比为4.7:2.6:1,半乳糖醛酸含量为26%。将SA先经部分酸水解,再经Smtch降解得到β-(1→3)-D-聚半乳糖。SB的组成以酸性糖为主,半乳糖醛酸含量为76%,半乳糖、阿拉伯糖、鼠李糖间的摩尔比为3.3:1.8:1。用部分酸水解方法,可从SB获得分子量小于2万的α-(1→4)-D-聚半乳糖醛酸。     

Chemical structure and biological activity of water-soluble polysaccharides from Cassia angustifolia leaves

The water-soluble polysaccharides from Cassia angustifolia L. leaves were isolated and fractionated. The acidic polysaccharide fraction was separated into two subfractions S1 and S2 consisting of L-rhamnose, L-arabinose, D-galactose, and D-galacturonic acid. Further fractionation of the predominant S1 by GPC gave two fractions S1A and S1B with an average molecular weight of 2 x 10(6) and 1.5 x 10(5) d, respectively. Methylation analysis of S1A showed the presence of 1,4-linked galacturonic acid (31.0%), 1,2-linked rhamnose (14.5%), 1,2,4-linked rhamnose (15.8%), 1,3,6-linked galactose (15.3%), smaller amounts of 1,3-linked arabinose, 1.5-linked arabinose, and terminal galactose and arabinose residues. Mild acid hydrolysis of S1A indicated that the backbone consists of 1,4-linked galacturonic acid and 1,2-linked rhamnose residues in the ratio of 1:1. Every second rhamnose is connected via C-4 to arabinogalactan sidechains. The antitumor activity of the polysaccharide fractions was tested against the solid Sarcoma-180 in CD1 mice. Only S1A exhibited a significant antitumor activity with an inhibition rate of 51%.