阴离子交换分离－脉冲安培检测分析糖类化合物的进展

 简述了糖的主要生物学作用及测定糖的主要方法，重点讨论了近年来建立起来的高效阴离子交换色谱－脉冲安培检测（ＨＰＡＥＣ－ＰＡＤ）技术。对此技术的基本理论、应用现状及优缺点进行了较为详细的叙述。     

ICP－AES法检测Sr、Ca、Mg、P在海带多糖中的分布

应用ＩＣＰ－ＡＥＳ技术，检测了Ｓｒ、Ｃａ、Ｍｇ、Ｐ在海带叶状体的褐藻淀粉、藻酸盐、褐藻糖胶和纤维素等多糖中的分布，发现锶主要存在于褐藻糖胶中［９．６×１０－３（糖干重），占叶状体总锶的４７．２％］，而其他成分中的锶含量都较低。提示锶与维持藻体结构有关。     

ICP—AES法检测Sr,Ca,Mg,P在海带多糖中的分布

应用ＩＣＰ－ＡＥＳ技术，检测了Ｓｒ，Ｃａ，Ｍｇ，Ｐ在海带叶状体的褐藻淀粉，藻酸盐，褐藻糖胶和纤维素等多糖中的分布，发现锶主要存在于褐藻糖胶中，而其他成分中的锶含量都较低，提示锶与维持藻体结构有关。     

海带细胞壁及细胞壁多糖中Sr,Ca,Mg,P分布

对海带细胞壁及细胞壁中的藻酸盐、褐藻糖胶、纤维素等多糖类物质中的Ｓｒ、Ｃａ、Ｍｇ、Ｐ含量作了ＩＣＰ－ＡＥＳ测定。结果显示，海带中的锶主要位于细胞壁，细胞壁中的锶主要位于揭藻糖胶。     

高效液相色谱法同时测定食品和药品中的糖及其降解产物5—羟甲基糠醛

５－羟甲基糠醛（５－ＨＭＦ）是糖的降解产物，本文提出了用高效液相色谱法同时测定食品和药品中的蔗糖，葡萄糖，果糖和５－ＨＭＦ的方法，采用氢型阳离子交换色谱法Ａｍｉｎｅｘ－ＨＰＸ－８７Ｈ，以乙腈－０．０１ｍｏｌ／Ｌ，硫酸（４０：６０）为流动相分离糖和５－ＨＭＦ，使用串联的紫外光度检测器（２８０ｎｍ）和示差折光检测器，分别检测５－ＨＭＦ和糖。     

铕与醛糖及铕与D—核糖,L—氨基酸络合作用的伏安法研究

Ｅｕ＾３＋在ＨＡｃ－ＮａＡｃ溶液中与五碳醛糖有弱的络合作用，用循环伏安法和微分脉冲极谱可以观察到Ｄ－核糖，Ｄ－阿拉伯糖，Ｄ－木糖对Ｅｕ＾３＋还原波形的络合影响，使还原和氧化过程变得较为可逆，其中Ｄ－核糖最为明显。而来苏糖无影响。Ｅｕ＾３＋与氨基酸在相同实验条件下的有络合作用，且在汞电极上有吸附现象，因此分别加入Ｌ－苯丙氨酸、Ｌ－组氨酸和Ｌ－蛋氨酸等，进一步改善了Ｅｕ＾３＋的波形而接近可逆氧化－还原     

烟草中糖类物质的高效毛细管电泳-安培检测研究

将高效毛细管电泳－安培检测技术（ＨＰＣＥ－ＡＤ）用于不同烟草样品中糖类物质的测定。在 １×１０－６ｍｏｌ／Ｌ～１×１０－３ ｍｏｌ／Ｌ范围内,存在良好的线性关系,葡萄糖、果糖、蔗糖和麦牙糖的检测限均小于 ５．０ ×１０－７ｍｏｌ／Ｌ,结果令人满意。     

高效液相色谱法分离和鉴别棉花中13种糖

应用一根Ｓｈｉｍ－ｐａｃｋＣＬＣ－ＮＨ２柱（６０ｍｍ×１５０ｍｍ）和一根Ｌｉｃｈｒｏｓｏｒｂ－ＮＨ２柱（５ｍｍ×２５０ｍｍ）串联组合，用ＲＩＤ－６Ａ折光检测器检测，以ＣＨ３ＣＮ＋Ｈ２Ｏ（７５＋２５）作流动相，成功地分离了鼠李糖、木糖、树胶醛糖、果糖、葡萄糖、半乳糖、蔗糖、纤维二糖、海藻糖、乳糖、蜜二糖、松三糖、棉籽糖，建立一种快速简便的测糖方法。     

铕与醛糖及铕与D─核糖、L─氨基酸络合作用的伏安法研究

Ｅｕ（３＋）在ＨＡｃ－ＮａＡｃ（ｐＨ４．６）溶液中与五碳醛糖有弱的络合作用，用循环伏安法和微分脉冲极谱可以观察到Ｄ－核糖，Ｄ－阿拉伯糖，Ｄ－木糖对Ｅｕ（３＋）还原波形的络合影响，使还原和氧化过程变得较为可逆，其中Ｄ－核糖最为明显，而来苏糖无影响．Ｅｕ（３＋）与氨基酸在相同实验条件下有络合作用，且在汞电极上有吸附现象，因此分别加入Ｌ－苯丙氨酸、Ｌ－组氨酸和Ｌ－蛋氨酸等，进一步改善了Ｅｕ（３＋）的波形而接近于可逆氧化－还原过程，其中以Ｅｕ（３＋）－Ｄ－核糖－Ｌ－苯丙氨酸最明确。绘出了在电极表面形成三元络合物的示意图。     

基体辅助激光解吸—电离飞行时间质谱法分析衍生化的寡链糖

以２，５－二羟基苯甲酸（ＤＨＢ）＋间硝基苄醇（ＮＢＡ）混合基体辅助激光解吸电离飞行时间质谱法（ＭＡＬＤＩ）分析甲壳素降解并衍生化的寡链糖，获得了满意的结果。对比其它基体，如：芥子酸（ＳＡ）、α－氰基－４－羟基肉桂酸等（α＿ＣＨＣＡ），２，５＿ＤＨＢ＋ＮＢＡ混合基体解吸电离效果最好：信号强、信噪比高。甲壳素降解产物的质谱分析至今未见报道。     

糖类化合物亲水作用色谱保留行为评价

以糖类化合物为研究对象,系统评价了其在亲水模式下的色谱保留行为。分别考察了流动相、固定相和缓冲盐等对糖类化合物保留的影响,建立了糖类化合物在亲水模式下的保留方程。结果表明,糖类化合物随着流动相中乙腈比例的降低,保留时间减小;随着缓冲盐浓度的增加,保留时间增加;同时,糖类化合物的保留行为还会受到有机溶剂种类和固定相类型的影响;其保留行为可使用顶替吸附-液相相互作用模型定量描述。将该模型进一步用于实际样品中糖类化合物保留行为的预测,获得了较好的实验结果,预测保留时间与实测保留时间的相对误差小于0.3%。对糖类化合物亲水模式下的保留行为进行了系统的评价和定量描述,该研究结果将有助于糖类化合物亲水作用色谱分离方法的发展。     

超高效液相色谱法测定卷烟烟丝中7种水溶性糖含量

以ACQUITY UPLC BEH Amide柱为分析柱,乙腈－0．2％三乙胺一水作为流动相,建立了超高效液相色谱－蒸发光散射检测器测定卷烟烟丝中鼠李糖、木糖、果糖、甘露糖、葡萄糖、蔗糖、麦芽糖7种水溶性糖的分析方法。7种水溶性糖回归方程的线性相关系数均大于0．999,检出限为0．56～1．11μg／mL。7种水溶糖的回收率在90．43％106．41％之间,相对标准偏差为1．66％－4．35％仰：6）。该方法灵敏度、准确度高,稳定性好,可用于大批量卷烟烟丝中水溶性糖含量的测定。     

Recent developments in capillary electrophoresis and capillary electrochromatography of carbohydrate species

This review article is concerned with the recent developments in capillary electrophoresis (CE) and capillary electrochromatography (CEC) of carbohydrates. The literature shows that CE possesses impressive potential in the analysis of carbohydrates. On the other hand, CEC has just started to show promise in the analysis of carbohydrates. Advances in separation and detection approaches of derivatized and underivatized carbohydrates are discussed based on the available literature. In addition, important applications are illustrated.     

糖合成中羟基的保护和去保护方法

糖中含有多个活泼的羟基.羟基的保护和去保护在有关糖的合成中具有很重要的意义.最常用的羟基保护基可归纳为三类:酯类、醚类和缩醛或缩酮类.作者对每一类中具体的羟基保护基的性质、应用作了简单综述,重点介绍了保护基的引入和脱去的方法.     

Organotin-catalyzed highly regioselective thiocarbonylation of nonprotected carbohydrates and synthesis of deoxy carbohydrates in a minimum number of steps

Nonprotected carbohydrates: The catalytic regioselective thiocarbonylation of carbohydrates by using organotin dichloride under mild conditions was demonstrated. The reaction afforded various deoxy saccharides in high yields and excellent regioselectivity in a minimum number of steps. The regioselectivity of the thiocarbonylation is attributed to the intrinsic character of the carbohydrates based on the stereorelationship of their hydroxy groups (see scheme).     

Simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection

A direct, sensitive, simple and practical method for simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection was developed. The retention behavior of amino acids and carbohydrates on the anion-exchange column and the detection of amino acids and carbohydrates at different integrated pulsed amperometric detection waveforms were investigated. The optimized gradient eluent conditions for analysis of 17 amino acids and nine carbohydrates were obtained. Separation time was 100 min. Detection limits for amino acids and carbohydrates were 5.2-207.1 nM under injection volume of 25 microl. The RSDs of peak area were 1.2-3.3%. The calibration graphs of peak area for the analytes were linear over about three orders of magnitude with a correlation coefficient of 0.9950-0.9999. The method was applied to determine amino acids and carbohydrates in a liquid condiment with satisfactory results.     

Derivatization Reaction of Carbohydrates with Urea as the Reagent and Fluorimetric Determination of Carbohydrates

ＩｎｔｒｏｄｕｃｔｉｏｎＣａｒｂｏｈｙｄｒａｔｅｓｐｌａｙａｎｅｓｓｅｎｔｉａｌｒｏｌｅｉｎｎａｔｕｒｅａｎｄａｌｍｏｓｔａｌｌｔｈｅｌｉｆｅｐｒｏｃｅｓｓｅｓ .Ｔｈｅｙａｒｅｎｏｔｏｎｌｙｃｅｎｔｒａｌｔｏｔｈｅｇｅｎｅｒａｔｉｏｎａｎｄｓｔｏｒａｇｅｏｆｅｎｅｒｇｙｂｕｔａｌｓｏｕｓｅｆｕｌｉｎｔｈｅｄｉａｇｎｏｓｉｓｏｆｄｉｓｅａｓｅｓａｎｄｄｙｎａｍｉｃａｄｊｕｓｔｍｅｎｔｆｏｒｔｈｅｆｕｎｃｔｉｏｎｓｏｆｐｒｏｔｅｉｎ .Ｓｏｅｓｔａｂｌｉｓｈｉｎｇｈｉｇｈｓｅｎｓｉｔｉｖｅａｎｄｅｆｆ…     

Influence of the tannin structure on the disruption effect of carbohydrates on protein-tannin aggregates

The disrupting effect of three different ionic carbohydrates (xanthan, pectin and gum arabic) on the formation of tannin-protein insoluble aggregates was assessed by nephelometry using bovine serum albumin (BSA) and several procyanidin fractions previously extracted from grape seeds. The presence in solution of any of the carbohydrates studied was found to restrain the formation of insoluble protein-tannin aggregates for every procyanidin fraction used. Xanthan was the most effective carbohydrate, whereas gum arabic was the least effective. The present work has revealed that the disrupting effect of carbohydrates is quite different depending on the procyanidin structure complexity. In general, the three carbohydrates studied revealed a similar trend in that their disrupting effect on tannin-BSA aggregate formation decreased with increase of the procyanidin degree of polymerization.     

Postcolumn derivatization for chromatographic analysis of carbohydrates

Various methods for postcolumn derivatization of carbohydrates for photometric (P), fluorimetric (F) and electrochemical (E) detection are summarized. The major methods include conversion to furfurals (with strong mineral acids, reducing carbohydrates, for P), formaldehyde (with periodate, carbohydrates in general, for P and F), glycamines (by reductive amination, reducing carbohydrates, for P and F), etc., followed by condensation with appropriate chromogenic or fluorogenic reagents; direct or indirect coloration of leuco compounds (for P) or chelating agents (for P and E), respectively, by utilizaing the reducibility of reducing carbohydrates; reactions with fluorogenic reagents such as aliphatic amines (for F), 2-cyanoacetamide (for P, F and E), arginine (for F), benzamidines (for F), etc., in neutral or weakly alkaline media; and coloration of the condensates with hydrazino compounds in alkali (for P). The characteristics features of individual methods and their optimized conditions are reviewed.     

Supercritical fluid chromatography of carbohydrates

Supercritical fluid chromatography (SFC) is a relatively new technique applied to polar solutes such as carbohydrates about 10 years ago. The developments in the SFC of carbohydrates are summarized and a comparison between capillary and packed column SFC is presented. High-efficiency capillary columns are suitable only for derivatized carbohydrates since various packed columns are well adapted for non derivatized mono-, di- and trisaccharides and provide complementary selectivities.