离子色谱法测定不同产地葛根多糖中的单糖组成

建立了葛根中岩藻糖、鼠李糖、阿拉伯糖、半乳糖、葡萄糖、甘露糖、木糖、核糖、甘露醇、木糖醇、果糖等11种单糖的离子色谱方法,并应用此方法分析了不同产地葛根多糖中单糖组成及含量。葛根多糖经超声提取,Box-Behnken响应面优化超声提取条件,三氟乙酸水解,以Carbo Pac PA20(150 mm×3 mm)色谱柱分离,20 mmol/L NaOH溶液等度洗脱。结果表明,11种单糖的定量限为0.03~0.07 mg/kg,在0.2~5 mg/L线性范围内线性关系良好(r~20.9990),加标回收率为80.3%~112.4%。经Box-Behnken响应面优化后的最佳提取工艺为液料比28:1(mL/g),超声时间44 min,超声温度65℃。经离子色谱方法测定不同产地的葛根样品中均含有岩藻糖、鼠李糖、葡萄糖,其中葡萄糖的含量最高含量在114.3~622.2 mg/g之间。方法可为葛根质量评价提供技术支撑。     

海水小球藻中多糖的提取及其单糖组成的气相色谱-质谱分析

在温度为70℃、功率为600 W、提取时间为30 m in的条件下,海水小球藻中的多糖可以得到较好的提取。经过优化,当超声波作用时间为90 m in、超声波功率为300 W、水解液为1 mol/L乙酸时,小球藻多糖的超声水解效果最好。碱提、水提、酸提海水小球藻多糖中的单糖组成,经过GC-MS分析,它们的单糖组成各不相同。碱提粗多糖中所含单糖为鼠李糖、L-岩藻糖、D-阿拉伯糖、D( )-木糖、D-甘露糖、D-葡萄糖、D-半乳糖,各单糖百分含量分别为20.68%、0.32%、1.0%、2.20%、4.58%、50.28%、20.91%(W/W);水提海水小球藻粗多糖中含鼠李糖、核糖、岩藻糖、阿拉伯糖、木糖、甘露糖、葡萄糖、半乳糖8种单糖,它们百分比分别为2.32、2.36、0.24、0.89、0.56、3.44、78.21、11.99%(W/W);酸提粗多糖中所含单糖为鼠李糖、核糖、岩藻糖、阿拉伯糖、木糖、甘露糖、葡萄糖、半乳糖,各单糖百分含量分别为2.75、1.75、0.23、1.04、0.61、5.99、74.33、13.30%(W/W)。本实验所建立的微波辅助提取、超声水解多糖、GC-MS分析多糖中的单糖组成等方法,具有简便、快速、准确的特点。可用于海藻和其它植物中的多糖研究。     

单糖立体异构体的测定: 正丁基硼酸衍生物的快原子轰击质谱

研究了把衍生化反应引用到正离子质谱中, 利用正丁基硼酸[n-BuB(OH)2]对自然界常见的11种单糖: D-核糖、D-来苏糖、D-木糖、L-阿拉伯糖、L-鼠李糖、L-岩藻糖、D-葡萄糖、D-甘露糖、D-半乳糖、D-果糖、L-山梨糖进行衍生化反应, 通过快原子轰击(FAB)谱图区分单糖的立体异构体, 以进一步探讨区分寡糖、多糖及糖甙化合物中糖的立体异构体的方法.     

气相色谱-质谱法分析研究野生菱角壳中多糖化合物的单糖组成

采用乙醇分级沉淀法，首次从野生菱角壳中提取出4种多糖化合物，利用气相色谱-质谱法，确定了菱角多糖分别由阿拉伯糖，鼠李糖，木糖，甘露糖，半乳糖，葡萄糖，乳糖和蜜二糖组成，其中以葡萄糖，半乳糖，甘露糖和木糖为主。     

毛细管电泳紫外检测法同时分析樟芝多糖水解液中8种单糖

本文报道了同时分析D-木糖、阿拉伯糖、葡萄糖、鼠李糖、D-甘露糖、半乳糖、D-葡萄糖醛酸和D-半乳糖醛酸8种单糖的毛细管电泳紫外检测方法。利用本研究所建立的方法,可以同时检测樟芝多糖水解液中的8种单糖,方法的检测限为0.11～0.22μg/mL,回收率在88%～104%之间,相对标准偏差(RSD)小于3%。本研究为分析表征樟芝多糖提供了一种可靠的方法。     

离子色谱-脉冲安培法测定芦荟多糖中7种单糖的含量

采用水提醇沉法提取芦荟鲜叶中的多糖，经三氟乙酸水解，利用Dionex CarboPac PA10高效阴离子色谱柱分离，氢氧化钠梯度淋洗，积分脉冲安培检测，建立了芦荟多糖中岩藻糖、鼠李糖、阿拉伯糖、半乳糖、葡萄糖、甘露糖和木糖7种常见单糖的测定方法。结果表明：7种单糖在线性范围内的相关系数（R²）均高于0.997，检出限为0.007~0.024 mg/L，加标回收率为97.5%~102.5%，相对标准偏差（RSD）为0.1%~4.8%。该法简单、快速、灵敏、准确，可用于芦荟多糖中单糖含量的测定和多糖组成的研究。     

高效阴离子交换色谱-脉冲安培法检测小鼠尿液中的甘露醇、单糖和乳果糖

采用高效阴离子交换色谱-脉冲安培检测法(HPAEC-PAD)建立了小鼠尿液中甘露醇、单糖(包括半乳糖、葡萄糖、甘露糖和果糖)和乳果糖的分析方法。样品经离心沉淀除去蛋白并过分子膜,以CarboPacTM PA1阴离子交换柱为分离柱,采用NaOH梯度淋洗,脉冲安培四电位检测。结果表明,甘露醇、半乳糖、葡萄糖、甘露糖、果糖和乳果糖在0.1～5.0 mg/L内线性良好,线性相关系数r2为0.988～0.999,样品加标回收率为95.5%～104.2%,检出限为0.0013～0.0048 mg/L。此法准确、快速、简便,能同时对6种糖类化合物进行分析,可以跟踪检测整个糖类代谢过程中甘露醇、单糖和乳果糖之间的代谢关系。     

柱前衍生化-高效液相色谱法分析木糖结晶母液的单糖组成

采用1-苯基-甲基-吡唑啉酮(PMP)柱前衍生化-反相高效液相色谱(HPLC)法建立了8种常见单糖的分离模式,并用于木糖结晶母液单糖组成的定量分析.结果表明:木糖结晶母液至少由甘露糖、鼠李糖、纤维二糖、葡萄糖、半乳糖、木糖、阿拉伯糖及岩藻糖8种单糖组成,其中以葡萄糖、半乳糖、木糖和阿拉伯糖为主.以峰高定量,8种单糖的浓...     

灵芝多糖的结构分析

从灵芝菌丝和子实体热水提取液中分离和纯化得到两种多糖，凝胶过滤导析测得分了量分别为３．７×１０＾４和４．２×１０＾４。气相色谱分析表明菌丝体多糖含Ｄ－葡萄糖，Ｄ－半乳糖，Ｄ－甘露糖，Ｄ－木糖，Ｌ－岩藻糖，Ｌ－鼠李糖，其摩尔比为５．３５：２．６７：１．００：１．１９：０．３８：０．３７；子实体多糖含Ｄ－葡萄糖，Ｄ－半乳糖，Ｄ－甘露糖，Ｄ－木糖，Ｌ－阿拉伯糖，Ｌ－鼠李糖，其摩尔比为５．８２：２．２３；     

纳米铜/石墨烯修饰电极用于离子交换色谱测定五种单糖

把纳米铜和石墨烯修饰在玻碳电极表面,制备了纳米铜/石墨烯复合修饰电极。采用电化学方法,在!1.5~0 V的循环扫描电位条件下,氧化石墨烯(GO)和Cu2+同时在玻碳电极上被电化学还原,形成石墨烯(Gr)和纳米铜(CuNPs)复合膜。所制备的修饰电极对葡萄糖等单糖化合物具有较高的电催化活性,且电极稳定性和重现性均良好。将此修饰电极作为电化学检测器,与高效阴离子交换色谱联用,分离测定了5种单糖化合物(岩藻糖、阿拉伯糖、半乳糖、葡萄糖和甘露糖)。结果表明,岩藻糖和阿拉伯糖的线性范围为0.1~100 mg/L,半乳糖、葡萄糖和甘露糖的线性范围为0.5~100 mg/L,5种单糖化合物的线性相关系数均大于0.998,相对标准偏差RSD(n=6)为1.9%~2.5%,检出限在0.02~0.10 mg/L之间;将此方法用于测定样品桑黄粗多糖的单糖组成,测得5种单糖的回收率为84.8%~94.5%,准确度和精密度均较好。     

用毛细管气相色谱法测定多糖中单糖的组成

报道了测定多糖中单糖组成的糖醇乙酸酯的毛细管气相色谱分析方法。使用ＯＶ－２２５毛细管气相色谱柱分离了１１种单糖的糖醇乙酸酯衍生物,在０．２～１．６８ｇ／Ｌ质量浓度范围内,１１种单糖定量校正曲线的线性关系廊。应用该法测定了胡麻我发多糖和少 我中单糖的组成。为这些药物多糖的基础研究提供了有用的信息。     

Determination of the compositions of polysaccharides from Chinese herbs by capillary zone electrophoresis with amperometric detection

In this paper, capillary zone electrophoresis with amperometric detection (CZE-AD) was applied to determine the compositions of hetero-polysaccharides from Chinese herbs, Angelica sinensis and flax by analyzing their hydrolyzed monosaccharides: fucose, galactose, glucose, arabinose, rhamnose and xylose. Under the selected optimum conditions, the six monosaccharides could be perfectly separated within 25 min and showed significant current responses at copper electrodes. The linear ranges of the six monosaccharides were all from 5.0 x 10(-6) to 2.0 x 10(-4) mol L(-1) and their detection limits were lower or near 1.0 x 10(-6) mol L(-1) (S/N = 3). Experiments showed that the Angelica sinensis polysaccharide was composed of fucose, galactose, glucose, arabinose, rhamnose and xylose (mole ratio 1.0:13.6:15.0:8.7:21.3:3.7), and the flax polysaccharide was composed of galactose, glucose and arabinose (mole ratio 1.0:4.98:1.1). The purity of these polysaccharides leached by the introduced leaching method was 98.3 and 97.6%, respectively. Analyzing polysaccharides by this method has some merits of speed, simple instrumentation and operation, high sensitivity and high reproducibility.     

Characterisation of natural polysaccharides (plant gums) used as binding media for artistic and historic works by capillary zone electrophoresis

The monosaccharide constituents of plant gums were separated by capillary electrophoresis at pH 12.1 and detected with indirect UV absorbance. The plant gums investigated were gum arabic, gum acacia, gum tragacanth, cherry gum and locust bean gum (carob gum). The monosaccharides obtained after hydrolysis with 2M trifluoroacetic acid and lyophilisation of the hydrolysate were arabinose, galactose, mannose, rhamnose, xylose, fucose, and glucose, and the two sugar acids galacturonic and glucuronic acid, in accordance with the literature. They were separated in a background electrolyte consisting of NaOH to adjust the pH, 20 mM 2,6-pyridinedicarboxylic acid as chromophore for detection and 0.5 mM cetyltrimethylammonium bromide as additive to reverse the electroosmotic flow. Based on their electropherograms, the plant gums could be identified by their typical composition (depicted in a decision scheme) as follows: a peak of glucuronic acid, together with that of rhamnose, is indicative for gum arabic. Peaks of galacturonic acid and fucose point to gum tragacanth. Locust bean gum shows a major peak for mannose (with the concomitant galactose peak in ratio 4-1), whereas a glucuronic acid and a mannose peak together with a prominent arabinose peak indicates cherry gum. The method was applied to identify the plant gums in samples like watercolours and in several paint layers like gum tempera or those with egg white or drying oils as additives. Artificial aging experiments of thin layers of gum arabic on paper or glass carried out with UV-A radiation (366 nm) did not result in changes of the saccharide patterns, in contrast to the simultaneously conducted aging of a drying oil layer.     

Glass capillary or fused-silica gas chromatography--mass spectrometry of several monosaccharides and related sugars: improved resolution

The gas chromatographic separation of several monosaccharides and related sugars derivatized by methoxylation and trimethylsilylation reactions was optimized with glass capillary (SP-2250) and fused silica (SP-2100) columns. Individual sugars included aldoses, ketoses, polyols, acidic forms and N-acetylated amino sugars. Peaks were detected by selected ion monitoring (SIM). The fused silica column gave complete resolution of all peaks (two per hexose and one per hexitol) arising from glucose, galactose, mannose, fructose, sorbitol, mannitol and dulcitol. The resolution of these sugars with the glass capillary column was not as good, but full differentiation was possible on the basis of SIM. Because the fused silica column gave a better resolution of 33 sugars tested and was more easily installed than the glass capillary column, it was utilized for quantitative analysis. A deuterated algal sugar mixture used for quantitation by isotope dilution was found to contain glucose, galactose, mannose, xylose, arabinose, ribose and rhamnose. Full recoveries were obtained of various amounts of glucose, galactose, mannose, fructose and xylose added to human serum.     

Separation of trimethylsilylated oximes of monosaccharides by capillary gas-liquid chromatography

Summary Trimethylsilylated oximes (TMS-oximes) of arabinose, fucose, galactose, glucose, mannose, rhamnose, xylose, glucuronic acid, and galacturonic acid were prepared using a two-step derivatization procedure. The TMS-oximes were separated and quantitated by gas-liquid chromatography using a 25-m fused-silica capillary column coated with crosslinked methylsilicone stationary phase. Starting with dried sugar extract, the entire procedure can be accomplished within 2 hours.     

Simultaneous analyses of neutral carbohydrates and amino sugars in freshwaters with HPLC-PAD

In this study, we determine concentrations of neutral and amino sugars and a sugar alcohol in freshwaters using high-performance liquid chromatography and pulsed amperometric detection with a single isocratic analysis. Coeluting arabinose, galactosamine, and mannosamine are separated with a mobile phase of 22.8 mM NaOH-KOH at a temperature of 17 degrees C. The resolutions are 0.73 and 0.64, respectively. The method separates closely eluting glucose-mannose and mannose-xylose peaks with resolutions of 0.85 and 0.71. Other sugars, fucose, rhamnose, galactose, fructose, ribose, glucosamine, and mannitol are resolved completely. Arabinose and galactosamine are measured in stream, ground, and soil waters that contain dissolved total saccharide (DTS) concentrations of 527 to 1555 nM. Failure to distinguish galactosamine from arabinose in those samples results in a 53-82% overestimation of arabinose concentrations and a 1.8-6.5% overestimation of DTS concentrations. The near unity of glucosamine and galactosamine concentrations in stream water samples allows us to suggest a correction factor for historical samples that had been analyzed without resolving galactosamine and arabinose.     

温和条件下柱前标记-高效液相色谱-质谱法测定枸杞多糖中单糖组成

基于高效液相色谱-质谱联用分析技术（HPLC-MS）,在温和的NH₃·H₂O条件下,采用1-苯基-3-甲基-5-吡唑啉酮（PMP）衍生化试剂成功地标记了果糖及多种醛单糖,同时提出了PMP标记果糖的衍生化机理。采用Kromasil-C18色谱柱（100 mm×4.6 mm,3.5 μm）分离,梯度洗脱,选择离子模式检测,建立了8种常见单糖标记物的结构确认及含量测定的分析方法。该方法在一定质量浓度范围内具有良好的线性（相关系数> 0.9947）,检出限为0.003~0.05 mg/L,定量限为0.01~0.15 mg/L。平均回收率为65.1%~116.2%,相对标准偏差≤10.2%（n=5）。自制4个产地枸杞多糖,对其单糖组成的分析结果表明,它们均由甘露糖、果糖、鼠李糖、半乳糖、葡萄糖、木糖、阿拉伯糖和脱氧核糖8种单糖组成,但各种单糖含量的分布有较大的差异。该法简便,灵敏度高,重复性好,可用于水热法水解枸杞多糖水解液中单糖标记物结构的确认及测定,对规范植物多糖的质量控制具有重要意义。     

半叶马尾藻粗糖中单糖的离子色谱法分析

以60～80 ℃的水从半叶马尾藻干粉中提取粗多糖,用Sevage溶剂去蛋白纯化后,将粗多糖用4.0 g/L 的三氟乙酸在 80 ℃下水解,水解液在CarboPacTM PA10离子色谱柱(2 mm i.d.×250 mm)上以14.0 mmol/L NaOH溶液为流动相进行 分离,以电化学检测器检测半叶马尾藻粗糖水解产生的单糖成分及含量。结果表明,半叶马尾藻粗糖中木糖、半乳糖、阿 拉伯糖、葡萄糖、鼠李糖和果糖的含量分别为2200,820,98,4560,358和740 mg/kg,加标回收率范围为86.0%~108.0%,检出限范围为5.6～89.6 μg/kg。该方法具有灵敏度高、精密度好、样品不需 要衍生化处理等优点,适合藻类样品中单糖的分析。