离子色谱法测定高山红景天多糖硫酸酯中硫酸根含量的研究

从高山红景天、平菇、红缘层孔菌中分别分离出多糖ＲＳＡ,ＡＴ,ＦＰ用氯磺酸吡啶法对多糖进行硫酸化修饰分别得到ＲＳＡＳＬ,ＡＴＳＬ,ＦＰＳＬ,多糖硫酸酯的生物活性与硫酸根的含量密切相关,用离子色谱法测定多糖硫酸酯中硫酸根的含量,ＲＳＡＳＬ为２７．７％,ＡＴＳＬ为３６．９２％,ＦＰＳＬ为３７．５％,与紫外比浊法相比,离子色７谱法具有准确、简便、重复性好等优点。     

生漆多糖的分离与结构研究

生漆用丙酮提取不溶解物，除去其水不溶部分、依次进行７３２阳离子交换树脂和ＳｅｐｈａｄｅｘＧ－１００柱层析、得到白色粉末漆多糖．分子量１２．５×１０￣４．其组成为Ｄ－半乳糖、Ｄ－葡萄糖醛酸、Ｌ－阿拉伯糖和Ｌ－鼠李糖．摩尔比为７．７：１．８：０．４：０．１．经羧基还原、甲基化反应、高碘酸盐氧化、Ｓｍｉｔｈ降解和ＧＣ－ＭＳ、ＩＲ、￣１Ｈ－ＮＭＲ、￣１３Ｃ－ＮＭＲ分析、结果表明，漆多糖为多分支结构、分子主链由β（１→３）Ｄ－半乳糖基构成．部分半乳糖基Ｃ＿６位有支链，另有部分半乳糖基以（１→６）键连接，其中β（１→３）与β（１→６）甙键糖基组成比为１．８３：１．分子的支链由葡萄糖醛酸基、阿拉伯糖基、鼠李糖基组成，并且葡萄糖醛酸基构成分子的末端基．     

在线流动注射液－液萃取系统在原子吸收光谱法中的研究及应用

本文对用于原子吸收光谱分析的在线液－液萃取流路系统进行了研究，采用了一种新型、适用、简便的相分隔器和相分离器，并用该流路系统对矿石、人发中的Ｃｕ（ＦＡＡＳ）以及矿石中痕量Ａｕ进行了测定（ＧＦＡＡＳ）。在水相和有机相的流量比为２５：１，采样频率为２０ｈ￣（－１）时，用ＦＡＡＳ法测定Ｃｕ的ＲＳＤ为１．９％（ｎ＝１０）、ＤＬ（３σ）为１．０μｇ．Ｌ￣（－１）；用ＧＦＡＡＳ法测定Ａｕ的ＲＳＤ为４．９％，ｎ＝１０、ＤＬ（３σ）为０．０８μｇ．Ｌ￣（－１）　。     

在线流动注射液—液萃取系统在原子吸收光谱法中的研究及应用

本对用于原子吸收光谱分析的在线液－液萃取流路系统进行了研究，采用了一种新型、适用、简便的相分隔器和相分离器，并用该流路系统对矿石、人发中的Ｃｕ（ＦＡＡＳ）以及矿石中痕量Ａｕ进行了测定（ＧＦＡＡＳ）。在水相和有机相的流量比为２５：１，采样频率为２０ｈ＾－１时，用ＦＡＡＳ法测定Ｃｕ的ＲＳＤ为１．９％（ｎ＝１０）、ＤＬ（３σ）为１．０μｇ·Ｌ＾－１；用ＧＦＡＡＳ法测定Ａｕ的ＲＳＤ为４．９％，ｎ＝１０、     

测定玻璃体和房水中维拉帕米含量的高效液相色谱法

研究了用ＨＰＬＣ 测定兔眼玻璃体和房水中维拉帕米含量的方法。用丙咪嗪为内标， 采用Ｓｐｈｅｒｉｃａｌ Ｃ１８色谱柱分离， 以甲醇－ ０ ．０４ ｍｏｌ／Ｌ 醋酸铵－ 乙腈－ 二乙胺（ 体积比１ ∶１ ∶０ ．５ ∶０ ．０２） 为流动相， 检测波长为２７８ｎｍ 。样品用正己烷－ 异丁醇提取后进样， 分析速度快。 样品及内标的保留时间分别为４ ．６３ ｍｉｎ 及９ ．２３ ｍｉｎ ； 线性范围为２ ．５ ～１００ ｍｇ／Ｌ， 相关系数ｒ 为０ ．９９９ ７ 。方法的回收率为１００ ．３ ％ （ ｎ ＝ ５） ，ＲＳＤ 为３ ．６３％ ， 日内ＲＳＤ 为０ ．５ ％ ～３ ．６１ ％ ， 日间ＲＳＤ 为３ ．７５ ％ ～４ ．８０ ％ ， 最低检测质量浓度为０．２５ ｍｇ／ Ｌ。 应用该法测定了创伤家兔玻璃体和房水中维拉帕米浓度的变化。     

沙棘果皮水溶性多糖Hn的结构研究

沙棘果皮水溶性多糖经酸性乙醇分级和ＤＥＡＥ－ＳｅｐｈａｄｅｘＡ－２５ｓｙｇｇ层析纯化,得到多糖Ｈｎ,经ＳｅｐｈａｒｏｓｅＣＬ－４Ｂ柱层析、玻璃纤维纸电泳、比旋光度测定等方法鉴定Ｈｎ为均一多糖。经唾液淀粉酶解、部分酸水解、高碘酸氧化、Ｓｍｉｔｈ降解、甲基化分析及ＩＲ,＾１３Ｃ－ＮＭＲ,ＧＣ和ＧＣ－ＭＳ等方法,确定其基本结构中主链由１→４ｌｃ基,１→６Ｍａｎ基和１→６Ｇａｌ基构成。三者摩尔比为ｎＧｌｃ     

HPLC法测定中成药制剂中10-羟基-2-癸烯酸的含量

采用ＳｐｈｅｒｉｓｏｒｂＣ１８柱,以甲醇∶水∶磷酸（４５∶６５∶０．５）为流动相,以ＵＶ２１０ｎｍ为检测波长,测定中成药制剂中１０－羟基－２－癸烯酸（１０－ＨＤＡ）的含量,１０－ＨＤＡ浓度在０．００６～０．０３０ｇ／Ｌ范围内线性关系良好（ｒ＝０．９９９９,ｎ＝５）,检测限为０．２ｍｇ／Ｌ（Ｓ／Ｎ＝３∶１）。方法具有定量准确、快速及主峰和杂质分离度高等特点。     

THE STUDY ON ELECTROXIDATION OF Fe（CN）_6~（4－） WITH TIME－RESOLVED IN FRARED SPECTRA

ＴＨＥ　ＳＴＵＤＹ　ＯＮ　ＥＬＥＣＴＲＯＸＩＤＡＴＩＯＮ　ＯＦ　Ｆｅ（ＣＮ）＿６￣（４－）　ＷＩＴＨ　ＴＩＭＥ－ＲＥＳＯＬＶＥＤ　ＩＮ　ＦＲＡＲＥＤ　ＳＰＥＣＴＲＡ￥ＹｏｎｇＹＡＮＧ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｆｏｒＰｈｙｓｉｃａｌＣｈｅｍ...     

RING ENLARGEMENT OF N-HETEROCYCLES

ＲＩＮＧＥＮＬＡＲＧＥＭＥＮＴＯＦＮ－ＨＥＴＥＲＯＣＹＣＬＥＳ￥ＪｉａｎＷｅｉＺＨＡＮＧ；ＪｉＹｕＧＵＯ；ＸｉａｏＴｉａｎＬＩＡＮＧ（ＩｎｓｔｉｔｕｔｅｏｆＭａｔｅｒｉａＭｅｄｉｃａ．ＣｈｉｎｅｓｅＡｃａｄｅｍｙｏｆＭｅｄｉｃａｌＳｃｉｅｎｃｅｓ．ａ...     

8—氮鸟嘌呤的极谱伏安行为

用循环伏安法（ＣＶ）、电流采样极诸法（ＳＣＰ，即ＴＡＳＴ）、常规脉冲极谱法（ＮＰＰ）、微分脉冲极谱法（ＤＰＰ）、线性扫描伏安法（ＬＳＶ）、Ｏｓｔｅｒｙｏｕｎｇ方波伏安法（ＯＳＷＶ）和计时库仑法（ＣＣ）等电化学技术研究了抗癌药物８－氮鸟嘌呤（８－ａｚａｇｕａｎｉｎｅ，ｇｕａｎａｚｏｌｏ，简称８－ＡＧ）的极谱伏安行为．在 ０． １ｍｏｌ／Ｌ Ｈ２ＳＯ４底液中，８－ＡＧ有一良好的还原峰，峰电位（Ｅｐ）在－０． ９５Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ，下同）附近，８－ＡＧ浓度在４×１０－６～８×１０－４ｍｏｌ／Ｌ范围内．峰高与浓度有良好的线性关系，线性相关系数ｒ＝０．９９９９～０．９９１０，检出限为１× １０－６ｍｏｌ／Ｌ．实验证明了该峰具有吸附性．本文提出了电极反应机理，它包括：酸性介质中８－ＡＧ的质子化、质子化的８－ＡＧ在汞电极上吸附以及完全不可逆的两电子还原过程．同时用量子化学计算方法（全略微分重叠法即ＣＮＤＯ／２）对８－ＡＧ和鸟嘌呤的各原子的净电荷以及Ｗｉｂｅｒｇ键级进行了计算，从理论上解释了８－ＡＧ的电化学还原机理。     

Structure Analysis of Pectin SB1-1 from the Root of Panax ginseng

A water-soluble pectin SB1-1 was isolated and purified from the root of Panax ginseng C. A. Mey. The HPLC analysis indicates that SB1-1 is homogenous. Its molecular weight was estimated via gel filtration to be 10000. The GC analysis indicated that it contains the monosaccharides of GalA, Gal, Ara and Rha. Their molar ratio is 2.10 : 1.00 : 0.12 : 0.13. Partial hydrolysis with acid, pectinase treatment, periodate oxidation, Smith degradation, methylation analyses, GC/MS analyses and NMR analyses were used for the structure analyses of SB1-1. The results reveal that SB1-1 has a lower branched structure. The main chain is composed of GalA and Gal; the inner part is a-1,4-linked-GalA; the border is 1,4-linked-Gal. Some of the 1,4-linked-GalA and 1.4-linked-Gal residues are substituted at O6. On an average, there is one branch for every ten hexose residues. The side chain is composed of 1,6-linked-Gal and 1,3,6-linked-Gal. The nonreduced end is composed of Rha, Ara and Gal. The main glycosidic link of SB1-1 has an a configuration.     

淫羊藿多糖的分子特征及免疫活性研究

用超声复合酶提取、离子交换凝胶分离、分子筛凝胶纯化得到3个淫羊藿叶多糖组分(EPs-1,EPs-2和EPs-3).3个多糖组分的分子特征通过气相色谱、高效凝胶渗透色谱进行了表征,并采用体外淋巴细胞增殖和巨噬细胞吞噬活性实验对多糖的免疫活性进行了评价.3个多糖组分EPs-1,EPs-2和EPs-3的总糖含量分别为90.36%,94.51%和89.19%.EPs-1,EPs-2和EPs-3主要由半乳糖醛酸(GalA)、半乳糖(Gal)、鼠李糖(Rha)、木糖(Xyl)、阿拉伯糖(Ara)和甘露糖(Man)组成,其平均相对分子质量分别为81.64×10~3,60.53×10~3,21.85×103;3个多糖都能够促进脾淋巴细胞增殖和激活巨噬细胞活性.这些结果说明淫羊藿多糖可以作为天然的免疫活性调节剂应用于医药和功能食品.     

白花蛇舌草免疫多糖结构的研究

白花蛇舌草(Hedgotis diffusa willd)系茜草科(Rubiaceae)耳草植物,民间常用此草内服治疗小儿疳疾、毒蛇咬伤、癌肿及肠道疾病,外用治疗各种疮疥及跌打刀伤等症.本文首次报道从白花蛇舌草水溶性成份中分离得到一个具有免疫活性的多糖,并对它的结构进行了初步的探讨.     

基于多孔石墨化碳柱-四极杆-飞行时间质谱解析甜菜果胶精细结构

采用高温酸法提取甜菜果胶(SBP), 经强阴离子交换柱层析分离, 获得甜菜果胶水洗脱组分(SBPW)和盐洗脱组分(SBP3). 单糖组成分析和分子量表征结果表明, SBPW主要由半乳糖(Gal)、 阿拉伯糖(Ara)和半乳糖醛酸(GalA)组成, 分子量为1100； SBP3则以GalA为主, 分子量为41450. 通过顺序酶法降解, 应用多孔石墨化碳柱-四极杆-飞行时间质谱(PGC-Triple-Tof MS)联用技术分析鉴定了SBPW和SBP3寡糖的精细结构. 结果表明, SPBW的主链为[→4)-α-GalA-(1→2)-α-Rha-(1→]重复单元构成的Ⅰ型聚鼠李半乳糖醛酸(RG-Ⅰ果胶), 鼠李糖O-4位被中性糖侧链[α-(1→5)阿拉伯聚糖和β-(1→4)半乳聚糖]所取代. SBP3由α-1,4链接的聚半乳糖醛酸(HG)和RG-Ⅰ构成, HG和RG-Ⅰ通过α-1,4糖苷键直接相连, 并发现了α-GalA(1→2)α-Rha(1→4)α-Rha(1→4)α-GalA(1→2)α-Rha的新特征结构.     

Ultrasonic-Assisted Aqueous Two-Phase Extraction and Properties of Water-Soluble Polysaccharides from Malus hupehensis

Malus hupehensis (M. hupehensis), an edible and medicinal plant with significant antioxidant and hypoglycemic activity, has been applied to new resource foods. However, the structural characterization and biological effects of its polysaccharides (MHP) are less known. The optimum extraction parameters to achieve the highest extraction efficiency (47.63%), the yield (1.68%) and purity of MHP (89.6%) by ultrasonic-assisted aqueous two-phase system (ATPS) were obtained under the liquid-to-solid ratio of 23 g/mL, ultrasonic power of 65 W, and ultrasonic time of 33 min. According to the analysis results, MHP was composed of Man, GlcA, Rha, GalA, Glc, Gal, Xyl, Ara, and Fuc, in which Ara and Gal were the main components, and the content of GlcA was the lowest. In in vitro activity analysis, MHP showed a significant antioxidant capacity, and an inhibition activity of α-glucosidase and the advanced glycation end products (AGEs) formation in the BSA/Glc reaction model. MHP interacted with α-glucosidase and changed the internal microenvironment of the enzyme, and inhibited the AGEs formation, which provides more evidence for the antihyperglycemic mechanism of MHP. The results suggest that ATPS is an efficient and environmentally friendly solvent system, and M. hupehensis has broad application prospects in functional foods, healthcare products, and pharmaceuticals.     

改性柑橘果胶的制备、表征及抗癌活性

采用琼脂糖凝胶电泳、比旋度测试、HPSEC-RID、IR、¹H NMR、¹³C NMR、高碘酸氧化及甲基化分析等手段对改性柑橘果胶(MCP)进行了分析, 结果表明, MCP是一种均一性多糖, 分子量约为21000~66000, 糖醛酸质量分数为81.0%, 酯化度为2.13%. MCP的中性单糖残基主要包括鼠李糖(Rha)、阿拉伯糖(Ara)、木糖(Xyl)和半乳糖(Gal)等, 其摩尔比约为1.0∶1.5∶1.4∶1.3, 主链包括HG和RG, 分支结构含有末端Gal, Xyl和Ara. 选用3种小鼠移植性肿瘤模型对MCP的抗肿瘤生长活性进行研究. 结果表明, MCP对肝癌H22细胞有较强抑制作用, 高剂量下抑制率可达47.8%; 对宫颈癌U14细胞的抑制率在高剂量及中等剂量下分别达到36.5%和38.5%; 对肉瘤S180没有抑制活性. MCP的抗肝癌和抗宫颈癌活性为首次发现.     

肉苁蓉茎水溶性多糖SPA的结构分析

肉苁蓉为稀有的名贵中药材 ,具有补肾、益精、润肠及抗衰老等功效 [1] .研究表明 ,肉苁蓉多糖具有延缓皮肤衰老、增强机体免疫功能、促进人体外成纤维细胞的生长及促进创伤愈合 [2 ] 等生理活性作用 .对于肉苁蓉多糖的深入研究尚未见报道 ,为探讨多糖的生物活性与结构的关系 ,本文对肉苁蓉茎水溶性多糖 SPA组分进行结构分析 .有关肉苁蓉茎水溶性多糖 SPA组分的分离纯化过程见文献 [3].1　实验部分1 .1　试剂与仪器　 Sephadex G- 75 ( Pharmacia公司 ) ;二甲基亚砜 (江苏洪声化工厂 ) ;Shimadzu高压液相色谱 (日本岛津 ) ;Vavian 340 0…     

枸杞子糖缀合物LbGp4糖链的结构及其免疫活性的研究

枸杞子糖缀合物LbGp4经β--消除、柱层析分离后得到一条分子量高达180800的分支多糖化合物LbGp4-OL.LbGp4-OL糖基组成为n(Rha):n(Ara):n(Gal)=0.05:1.33:1.根据甲基化、部分酸水解及¹HNMR、¹³CNMR分析,确定了其主要的结构,并对LbGp4和LbGp4-OL的免疫活性进行了研究.     

Molecular properties and immunomodulatory activities of a water-soluble heteropolysaccharide isolated from Plantago asiatica L. leaves

This study aims at investigating physical–chemical properties of a water-soluble heteropolysaccharide from Plnatago asiatica L. leaves, and its immunomodulatory effects on macrophages RAW264.7 cells. Hot water-extracted crude polysaccharide from the plant leaves (PLLCP) was fractionated into four fractions by DEAE Sepharose Fast Flow eluted with 0.1–0.5 M NaCl solutions. The most abundant fraction (0.3 M NaCl elution), designated PLLP-2, was identified as a heteropolysaccharide with an average molecular weight (M_w) of 3.54 × 10⁴ and composed mainly of Gal (34.4%), GalA (36.5%), Ara (10.1%) and Rha (8.4%). PLLP-2 was an acidic polysaccharide exhibiting inflaky curly aggregation with smooth surface. PLLCP and its main subfraction PLLP-2 displayed immunomodulatory activities by stimulating the production of pro-inflammatory cytokines, including TNF-α and IL-1β in macrophage RAW264.7 cells. These results indicate that the main polysaccharide fraction purified from P. asiatica L. leaves is probably pectin, and have potential immunomodulatory function.     

Physico‐chemical Properties and Bioactivities of a Glycoconjugate LbGp5B from Lycium barbarum L

A glycoconjugate designated as LbGp5B was isolated from the fruit of Lycium barbarian L. and purified to homogeneity by gel filtration. LbGpSB is composed of rhamnose (Una), arabinose (Ara), galactose (Gal), glucose (Glc), galacturonic add (GalA) and seventeen amino adds. The molecular weight of LbGpSB was determined by sodium dodecyl sulfate‐polyacrylamide gel electrophoresis (SDS‐PAGE) and by matrix‐assisted laser desorption/ionization (MALDI) time of fight (TOF) mass spectrometry (MS). The preliminary experiments showed that LbGpSB promoted splenocyte proliferation in mice and inhibited the peroxidation of low density lipoprotein (LDL).