麻风树叶多糖的分离纯化及组成分析

使用DEAE-纤维素、活性炭脱色和凝胶过滤色谱从麻风树叶粗多糖中纯化得到了两种多糖组分(JLP-3-1和JLP-3-2),经过高效凝胶渗透色谱分析,它们为均一多糖,相对分子质量为3.2968×106、1.8152×106Da左右。IR和HPLC分析表明,两组分(JLP-3-1和JLP-3-2)单糖主要是鼠李糖、果糖、半乳糖,也含有少量半乳糖醛酸。     

胶网藻多糖分离纯化、化学组成及其抗氧化活性

研究胶网藻（Dictyosphaerium sp.1A10）多糖的抗氧化活性并分析多糖的基本结构特征。采用超声辅助提取法对胶网藻多糖进行提取，并用DEAE-52纤维素柱层析和Sepharose CL-6B凝胶柱层析对粗多糖进行分离纯化，测定其 2，2-二苯基-1-苦基肼 [2，2-diphenyl-1-picrylhydrazyl，DPPH]、2，2''-联氮-双-3-乙基苯并噻唑啉-6-磺酸 [2，2''-Azinobis-（3-ethylbenzthiazoline-6-sulphonate），ABTS]、羟自由基清除率和还原能力，通过紫外光谱（ultraviolet spectrum，UV）、红外光谱（infrared spectrum，IR）、高效液相色谱（high performance liquid chromatography，HPLC）和高效凝胶色谱（high performance gel permeation chromatography，HPGPC）等技术进行基本结构分析。结果表明：（1）经过DEAE-52纤维素柱层析分离得到4个组分PC-1、PC-2、PC-3和PC-4，对抗氧化活性较高的多糖组分PC-4进行Sepharose CL-6B凝胶柱层析进一步纯化得到PCP-4；（2）胶网藻纯化多糖组分PC-4、PCP-4均具有一定的抗氧化能力；（3）胶网藻纯化多糖组分PCP-4的重均分子量（weight average molecular weight，Mw）为121 762 Da。多糖组分PCP-4含有吡喃糖和硫酸基。多糖组分PCP-4主要由鼠李糖、甘露糖和半乳糖醛酸组成，还有少量的葡萄糖醛酸、葡萄糖和半乳糖。     

三角帆蚌多糖的纯化工艺研究

利用离子交换及凝胶过滤层析方法对三角帆蚌粗多糖进行分离纯化.试验结果表明:采用弱阴离子交换色谱分离三角帆蚌粗多糖,用0.05 mol/L pH 7.9的Tris-HCl缓冲液以及0.1、0.2、1 mol/L NaCl洗脱液进行分段洗脱,得到4个组分;多糖含量较高的前2个组分经Sepharose 6B凝胶纯化,用双蒸水洗脱到2个组分,分别命名为MPa-1-1和MPa-2-1:经醋酸纤维素薄膜电泳法和高效液相凝胶色谱法鉴定,两者为均一纯多糖,测得MPa-1-1的分子质量为1589.62 kDa,MPa-2-1的分子质量为1741.80 kDa.     

红阳猕猴桃多糖组分的分离纯化、单糖组成及其抑制癌细胞活性

研究红阳猕猴桃果实多糖组分的分离纯化、单糖组成及其对癌细胞增殖的抑制作用。用水提取总多糖,层析法分离纯化多糖组分;高效凝胶渗透色谱测定组分的纯度和分子质量;高效液相色谱法测定多糖纯组分的单糖组成;傅里叶变换红外(Fourier transform-infrared,FT-IR)光谱鉴定多糖纯组分的特征官能团;用3-(4,5-二甲基噻唑-2)-2,5-二苯基四氮唑溴盐法测定多糖纯组分对肺癌、乳腺癌、肝癌、胃癌和结肠癌这5种癌细胞的体外抑制活性。总多糖分离出ACP-1、ACP-2、ACP-3、ACP-4这4种单组分多糖;其中ACP-3纯度最高,分子质量为2 663 k D,主要含有L-鼠李糖(17.78%,物质的量分数,后同)、D-半乳糖醛酸(25.25%)、D-半乳糖(25.45%)、L-阿拉伯糖(20.51%)、D-葡萄糖(6.14%)、D-甘露糖(2.13%)、D-木糖(1.03%)、D-葡萄糖醛酸(0.97%)及少量D-岩藻糖(0.74%);其FT-IR光谱图有多糖特征官能团的吸收峰。ACP-3对5种癌细胞增殖的半数最大抑制浓度依次为0.646、0.310、0.642、0.281、0.575μmol/L,对癌细胞增殖有抑制活性。     

南海鸢乌贼墨汁多糖分离纯化及组分分析

目的:从南海鸢乌贼墨汁中分离纯化多糖,并分析其多糖组分。方法:利用水提醇沉法得粗多糖,通过固相萃取层析法除色素对多糖进行纯化,纯化多糖依次经DEAE-52离子交换柱、Sephacryl HR-300凝胶柱分级纯化,按峰收集得单一组分,采用1-苯基-3-甲基-5-吡唑啉酮(1-phenyl-3-methyl-5-pyrazolone,PMP)衍生化方法,通过超高效液相色谱分析多糖组分。结果:粗多糖经DEAE-52离子交换柱、Sephacryl HR-300凝胶柱后收集得到3个糖组分,分别为SIP1、SIP2、SIP3;通过PMP衍生化方法分析单糖组成,得:SIP1是由D-甘露糖、D-葡萄糖、D-半乳糖3种单糖缩合而成;SIP2和SIP3分别是由D-甘露糖、鼠李糖、D-葡萄糖、D-半乳糖及L-(-)-岩藻糖5种单糖按照不同比例缩合而成。     

软枣猕猴桃多糖的分离与纯化及其分子质量的测定

对通过水提醇沉法提取、Sevag法脱蛋白得到的软枣猕猴桃多糖进行分离纯化,利用DEAE-纤维素52离子交换层析对软枣猕猴桃多糖进行初步分离,得到4种软枣猕猴桃多糖组分;利用葡聚糖凝胶对软枣猕猴桃多糖组分进一步分离的最佳条件为葡聚糖凝胶型号为Sephadex G-200、层析柱规格为D1.1cm×100cm、多糖质量浓度为10g/L。以此条件分离,得到含量较高的软枣猕猴桃多糖-Ⅱ纯品。通过Sephadex G-200凝胶柱层析鉴定软枣猕猴桃多糖-Ⅱ是均一的纯多糖,通过紫外光谱鉴定软枣猕猴桃多糖-Ⅱ不含核酸及蛋白。同时测得软枣猕猴桃多糖-Ⅱ的分子质量为83733D。     

蛹虫草菌糠多糖的分离纯化及结构组成分析

以蛹虫草菌糠为原料,利用纤维素酶酶解提取多糖,通过乙醇分级醇沉与Sevag法脱蛋白对所提多糖进行初级分离纯化,得到4 种多糖（P1、P2、P3、P4）。利用凝胶色谱、气相色谱-质谱联用技术（gas chromatographymassspectrometry,GC-MS）对这4 种多糖的分子质量分布与单糖组成进行分析;进一步利用Superdex 200凝胶柱层析对P2进行纯化精制,通过高碘酸钠氧化、Smith降解、红外光谱和核磁共振（nuclear magnetic resonance,NMR）技术表征了精多糖P2的一级结构。结果表明：乙醇分级沉淀与Sevag脱蛋白方法的结合能满足蛹虫草菌糠多糖初级纯化的要求,得到了较纯的P2、P3、P4组分,分子质量分别为35.9、9.4、3.7 kD;其中P2是由葡萄糖组成的葡聚糖,其主链结构主要为α-（1→4）吡喃葡聚糖。P3和P4是由甘露糖、葡萄糖和半乳糖组成的杂多糖,且单糖组成均以葡萄糖为主。     

胀果甘草酸性多糖的分离纯化、结构分析及免疫活性测定

目的分离纯化胀果甘草多糖,并对得到的3种酸性多糖组分结构及免疫活性进行分析。方法采用水提醇沉法提取胀果甘草粗多糖,经离子交换柱层析和凝胶柱层析分离纯化,高效凝胶渗透色谱法(high performance gel permeation chromatography,HPGPC)、红外光谱法(infrared spectroscopy,IR)、气相色谱法(gas chromatography,GC)和气相-质谱法(gas chromatography-mass spectrometry,GC-MS)分析其结构,采用H~3-胸腺嘧啶核苷掺入法(H~3-Td R)测定其对小鼠淋巴细胞增殖的影响。结果胀果甘草根及根茎经水提醇沉、离子交换柱层析和凝胶柱层析分离纯化后,得到3种相对分子量大于2.0×10~6 Da的均一酸性多糖组分Gi P-B1、Gi P-C1和Gi P-D1。结构和免疫活性的研究结果表明,这3种多糖组分均是由阿拉伯糖(Ara)、鼠李糖(Rha)、半乳糖(Gal)、半乳糖醛酸(Gal A)以不同摩尔比组成的酸性杂多糖,多糖的主链均由1,4-Galp A和1,2-Rhap残基构成,支链由1,5-连接的Araf和1,3-连接的Galp构成,支链分支点位于Rhap残基的O-4位。3种多糖在体外对小鼠脾细胞增殖均有促进作用,与空白对照组均有显著性差异(P0.05),其中糖醛酸含量最高的Gi P-D1促脾细胞增殖作用最高。结论从胀果甘草中分离纯化的3种酸性多糖为均一组分,具有一定的免疫增强活性。     

黄伞子实体多糖PAP2的分离纯化及其结构初步鉴定

从黄伞子实体中提取出水溶性粗多糖,经DEAE Sepharose Fast Flow和SuperdexTM 200柱层析分离纯化得到一种多糖组分PAP2。采用高效凝胶渗透色谱法(HPGPC)检测其为均一多糖组分,平均分子质量为2.1×106u;经高效液相色谱-蒸发光散射(HPLC-ESLD)检测表明PAP2主要由葡萄糖组成;结合红外光谱、核磁共振1H NMR和13C NMR分析表明,黄伞子实体多糖PAP2是一种α-D-吡喃葡聚糖,主链为1-4糖苷键,存在1-6糖苷键的支链。     

三叶青根多糖提取工艺优化、分离纯化及结构表征

采用水浴提取三叶青根多糖(Polysaccharides from roots of Radix Tetrastigma,RTP),以多糖提取得率为响应指标,在单因素试验的基础上,通过响应面分析方法确定三叶青根多糖提取的最佳工艺为:提取温度96℃、液料比34:1(mL/g)、提取时间2h,该条件下三叶青根多糖提取得率为(21.23±0.77)%。通过Sevage法除蛋白,并依次经DEAE-52离子交换柱、Sepharose CL-4B凝胶柱分级纯化,得到组分RTP-3-1。高效液相凝胶渗透色谱分析RTP-3-1为高纯度多糖,其分子量为1 244.2kDa,傅里叶红外光谱分析显示RTP-3-1是酸性多糖,核磁共振氢谱显示RTP-3-1为α型多糖。     

四氢呋喃衍生物的合成研究

本文以α-蒎烯为原料合成了2.2.5-三甲基-3-(3-甲基-2-丁烯基)四氢呋喃(4a)和2.2-二甲基-5-乙基-3-(3-甲基-2-戊烯基)四氢呋喃(4b)。化合物4a、4b具有幽雅的花香木香香韵,其卷烟加香试验表明:它们具有增加烟气浓度、使烟气团和细腻、改善口感的作用,是一类较为理想的烟用添加剂。      

Enzymatic Synthesis and Structural Confirmation of Novel Oligosaccharide,D-Fructofuranose-linked Chitin Oligosaccharide

Utilizing transglycosylation reaction catalyzed by β- N -acetylhexosaminidase of Stenotrophomonas maltophilia , β-D-fructofuranosyl-(2↔1)-α- N , N ´diacetylchitobioside (GlcNAc ₂ -Fru) was synthesized from N -acetylsucrosamine and N , N ´-diacetylchitobiose (GlcNAc ₂ ), and β-D-fructofuranosyl-(2↔1)-α- N , N ´, N ´´-triacetylchitotrioside (GlcNAc ₃ -Fru) was synthesized from GlcNAc ₂ -Fru and GlcNAc ₂ . Through purification by charcoal column chromatography, pure GlcNAc ₂ -Fru and GlcNAc ₃ -Fru were obtained in molar yields of 33.0 % and 11.7 % from GlcNAc ₂ , respectively. The structures of these oligosaccharides were confirmed by comparing instrumental analysis data of fragments obtained by enzymatic hydrolysis and acid hydrolysis of them with known data of these fragments.     

两种工艺芝麻油中挥发性风味物质的鉴别分析

旨在从不同芝麻油成品中找出共有的挥发性成分,为芝麻油掺伪鉴别提供数据支持。采用顶空固相微萃取-气相色谱-质谱法检测市售的压榨与水代法两种加工工艺生产的共10个品牌一级芝麻油中的挥发性风味物质,分析鉴别两种工艺芝麻油中共有的挥发性成分。结果表明：7个品牌压榨芝麻油中共检出49种风味物质,其中16种为共有成分,主要为酚类、吡嗪类、醇类、酮类、吡咯类、吡啶类等化合物;3个品牌水代法芝麻油中共检出61种风味物质,其中30种为共有成分,主要为酚类、吡嗪类、酮类、吡啶类、吡咯类、醇类、醛类等化合物;两种工艺生产的芝麻油中存在13种共有挥发性成分,分别为愈创木酚、芝麻酚、2-甲基吡嗪、3-乙基-2,5-二甲基吡嗪、2-乙基-6-甲基吡嗪、2-羟基-5-甲基苯乙酮、1-(5-甲基吡嗪-2-基)-乙酮、5-甲基呋喃醛、2-吡咯甲醛、3-糠醛、(1S,2S)-1,2-二(吡啶-4-基)乙烷-1,2-二醇、2-乙酰基吡咯、3-呋喃甲醇。综上,不同工艺、品牌芝麻油中存在共有挥发性成分,可作为芝麻油的特征标志物,用于芝麻油掺伪鉴别分析。     

分枝杆菌降解甾醇发酵生产雄烯二酮的两相系统培养基优化

对分枝杆菌Mycobacterium sp.BD696-6降解甾醇发酵生产雄烯二酮(AD)的两相系统培养基进行了优化。在甾醇添加量为0.6%时,培养基组成为有机相葵花油浓度20%、碳源糖蜜6%、氮源NH4NO30.3%、磷酸盐(NH4)2HPO40.08%条件下,AD得率最高,达到78.6%,比原培养基条件下得率提高了17.0%。     

去苦味冷溶型速溶绿茶的加工工艺

采用30 000、8000、3500、1000 u的有机膜,对绿茶浸提液进行超滤,以研究不同截留分子质量的膜管对绿茶浸提液中主要成分的分离和富集效应,以及对速溶绿茶品质的影响。结果表明,超滤绿茶汤时,以膜滤过程的膜滤时间、温度、超滤膜截留分子质量、压力对膜通量进行回归分析,可得到膜通量对膜滤时间、温度、超滤膜截留分子质量、压力的回归方程为-5.157 8-0.001 41+0.001 7X_2+0.000 1X_3+5.082 3X_4。其中,X_1为膜滤时间,0min≤X_1≤126min;X_2为膜滤温度,17.8℃≤X_2≤40℃;X_3为超滤膜截留分子质量,3500u≤X_3≤30 000 u;X_4为膜进口压力,31.5Pa≤X_4≤116.55Pa,由此可预测截留分子量在方程适合范围内的超滤膜的超滤过程。由截留分子质量为8 000u、1000u 2支超滤膜管组合使用所得的1000截留液样品,既具有冷溶性,又去除了苦涩味,茶汤的色、香、味俱佳。     

白鲢鱼肌原纤维蛋白双向电泳分析体系的建立

以白鲢鱼为研究对象,建立并优化其肌原纤维蛋白的双向电泳技术。结果表明,选用固相p H值梯度预制胶条p H 4~7,上样量120μg,等电聚焦程序Ⅲ(50 V主动水化15 h,250 V、2 h,1 000 V、2.5 h及4 000 V、3 h三段式除盐,8 000 V、2 h和10 000 V、1.5 h两段式升压,10 000 V聚焦80 000 V·h,500 V保持10 h)以及12%的十二烷基硫酸钠-聚丙烯酰胺凝胶电泳分离胶条件下进行双向电泳,凝胶银染后用PDQuest软件分析,得到具有高分离度的肌原纤维蛋白双向电泳图谱,蛋白点清晰。     

Eco-friendly methodologies for the synthesis of some aromatic esters, well-known cosmetic ingredients

Solid-liquid solvent-free phase transfer catalysis (PTC) and acidic catalysis in dry media were applied, with noticeable improvement and simplification over classical procedures in a Green Chemistry context, to the synthesis of some aromatic esters useful as cosmetic ingredients: 3-methylbutyl 4-methoxycinnamate, 2-ethylhexyl 4-methoxycinnamate, 2-ethylhexyl 4-(dimethylamino)benzoate and 2-ethylhexyl salicylate, well-known ultraviolet B sunscreen filters; 4-isopropylbenzyl salicylate, UV absorber and cutaneous antilipoperoxidant; propyl 4-hydroxybenzoate and butyl 4-hydroxybenzoate (parabens), antimicrobial agents. The reactions were performed under microwave (MW) activation and conventional heating. The best results for the synthesis of cinnamic, salicylic and 4-(dimethylamino)benzoic esters were achieved by in situ preformed carboxylates alkylation with alkyl bromides using PTC. The 4-hydroxybenzoates were obtained in good yields by classical esterification of the acid with alcohols using a simple heterogeneous mixture of reagents with catalytic amounts of p-toluenesulfonic acid (PTSA). The comparisons of yields and thermal profiles under either MW or conventional heating were studied and reported.     

4-(1-Phenylethyl)1,3-Benzenediol: A New, Highly Efficient Lightening Agent

There is an increasing world-wide demand for skin lightening active ingredients. Many common lightening ingredients on the market are either unsafe or ineffective at low concentrations. We therefore screened a series of hydroxy-stilbene derivatives for tyrosinase inhibitory activity. By chemical synthesis, the structures were optimized for efficacy and stability. The final candidate, 4-(1-phenylethyl)1,3-benzenediol, was found to be stable and to inhibit mushroom tyrosinase 22 times more effectively than kojic acid. In an assay with B16V melanoma cells, 4-(1-phenylethyl)1,3-benzenediol was the most potent inhibitor of melanin synthesis with an IC₅₀ of 2 μM among the compounds investigated. The lightening effect of 4-(1-phenylethyl)1,3-benzenediol was not due to cytotoxicity as proved by an MTT assay on B16V cells. On pigmented 3D epidermis models, 0.1% of 4-(1-phenylethyl)1,3-benzenediol led to an almost complete suppression of melanin synthesis after 14 days of incubation. Finally, an in vivo test on Asian subjects proved that 4-(1-phenylethyl)1,3-benzenediol efficiently lightens human skin at 0.5% dosage. Optimal results are achieved when 4-(1-phenylethyl)1,3-benzenediol is applied in formulations with low oil content. In summary, we have demonstrated that 4-(1-phenylethyl)1,3-benzenediol is a potent, stable and safe skin lightener.     

Structure,conformation and immunomodulatory activity of a polysaccharide from Morchella sextelata

Fungal polysaccharides are novel ingredients in functional foods with diverse medicinal properties. Here, a polysaccharide, MSP2-1, was isolated from Morchella sextelata fruiting bodies and purified using column chromatography. MSP2-1 (371.5 kDa) is a branched (1 → 4)-α-D-glucan with the O-6 or O-3 position occupied by α-D-Glcp. Light scattering analysis revealed that MSP2-1 has a spherical conformation in 0.9% NaCl solution; this was confirmed using transmission electron microscopy. Finally, MPS2-1 was found to promote proliferation, NO release and cytokine secretion in RAW264.7 cells through a mechanism involving Toll-like receptor 4. Collectively, these results highlight the potential application of MSP2-1 as an immunoenhancing compound for hypoimmunity.     

Dairy Ingredients effects on sausage sensory properties studied by principal component analysis

The effects of dairy ingredients (1, 3, 5%)–ordinary and high-viscosity sodium caseinate, skim-milk powder, whey protein or demineralized whey powder–on sensory properties and instrumental texture and color of sausages, were investigated. Sausages were formulated with 2 or 4% potato starch and cooked to a core temperature of 76 or 82°C. Principal component analysis (PCA) revealed three dominating factors for sensory properties; the first related to dairy ingredients and starch concentrations, the two others to type of dairy ingredients. Results were verified by analysis of variance (ANOVA). Results of sensory analysis were further verified by textural and color analysis using PCA and ANOVA, respectively.