木质纤维素类生物质超低酸水解试验及产物分析研究

在自行设计的木质纤维素类生物质超低酸水解装置上,结合以木聚糖和定量滤纸为模化物得到的半纤维素和纤维素水解的最佳工况,对白松、速生杨和玉米秸秆这三种在我国分布较为广泛的木质纤维素类生物质原料进行了高压液态水和超低酸水解相结合的两步水解研究,分别得到41．78％、57．84%和53．44％的原料转化率和39．28％、42．83％和23．82％的总还原糖转化率,并以HPLC定性了糖类产物,对产物中的低聚糖和单糖含量傲了对比,最后对速生杨水解残渣做了分析。     

小西瓜糖度表征与漫反射近红外检测方法的研究

研究小西瓜内部糖度分布规律的基础上提出了采用平均糖度、最高糖度和最低糖度表征小西瓜糖度的新方法。并采用便携式漫反射近红外分析仪,建立了快速测定小西瓜平均糖度,最高糖度和最低糖度近红外检测方法。最后将近红外检测方法与参考方法精度作了对比,结果表明漫反射近红外测量小西瓜糖度具有可行性。     

Synthesis of the deuterated thymidine-d9 and deuterated oligonucleotides

The efficient synthesis of the highly-deuterated thymidine-d₉ by the glycosylation reaction between a deuterated nucleobase and deuterated sugar is described. It is also incorporated into the oligonucleotides using a DNA synthesizer. Using this approach, it is possible to make highly-deuterated oligonucleotides for biological studies and structural analyses.     

NMR relaxometry study of gelatin based low-calorie soft candies

ABSTRACT

Soft candies are popular confectionery products. The most significant concern on the consumption of these products is the high amount of sugar and thus the high calories. The use of low-calorie sweeteners is a desirable trend in confectionery research. In this study, gelatin-based soft candies were formulated by using different sweeteners and their characterisation was performed using high and low field nuclear magnetic resonance (NMR) relaxation experiments. To complement the information obtained by NMR experiments, moisture content, water activity, texture analysis and differential scanning calorimeter experiments were also conducted. T₁ and T₂ relaxation times were measured at both low and high fields and also temperature-dependent measurements were conducted at the high field system. Candies were formulated by substitution of sucrose with maltitol, isomalt and stevia at 30%, 50% and 70% ratios. Significant difference was observed on relaxation times. T₁ values were best described by a mono-exponential model, whereas for T₂ relaxation times a bi-exponential model gave better results at both fields.     

LSSVM模型下的近红外光谱联合区间波长筛选方法

针对传统近红外光谱波长选择方法忽略模型中非线性因素的缺陷,采用具有非线性处理能力的最小二乘支持向量机,结合间隔策略的波长选择方法和联合区间的思想,提出了一种非线性模型下的波长筛选算法—联合区间最小二乘支持向量机(synergy interval least squares support vector machines, siLSSVM)。以苹果糖度近红外光谱数据为例,与传统siPLS波长筛选方法相比,新算法的预测集均方根误差(RMSEP)在PLS模型和LSSVM模型预测时分别提高了37.43%和47.88%,预测集相关系数(RP)在PLS模型和LSSVM模型预测时分别增加了6.04%和7.31%。实例表明,对于存在非线性因素较强的光谱数据,siLSSVM算法能够有效的挑选最优波长区间与提高模型的预测精度和鲁棒性,为近红外光谱在非线性因素下筛选波长提供了新前景。     

新型糖氨基酸类化合物的合成研究

糖氨基酸(sugar amino acids, SAAs)是一类同时含有氨基和羧基的糖类衍生物, 具有糖和氨基酸的结构特征和化学反应特性, 常作为多功能合成砌块用于组合化学的研究、糖模拟物和多肽模拟物的构建等. 因此, 该类化合物的设计与合成受到国内外化学家的持续关注. 在本文中, 我们发展了一种简单、高效的合成新型糖氨基酸的方法, 从廉价易得的3,4,6-O-三乙酰基-D-葡萄糖烯和3,4,6-O-三乙酰基-D-半乳糖烯出发, 在硝酸铈铵(CAN)的作用下通过一步自由基加成反应分别得到2-C-二羧酸酯类化合物gluco-2和galacto-2, 再经过脱羧、脱乙酰、碘代、叠氮化钠取代和一锅法还原氨化反应, 以最短直线步骤6步实现了糖氨基酸gluco-7(总收率34%)和galacto-7(总收率19%)的合成. 所有合成的化合物均经过IR, ¹H NMR, ¹³C NMR和HRMS的表征.     

木糖醇和麦芽糖醇型亲水作用色谱固定相的制备及其分离性能的评价

利用-NCO和-OH的加成反应,通过简单的两步反应将木糖醇和麦芽糖醇成功地键合于硅胶表面,制备了两种新型糖醇类亲水作用色谱固定相。流动相中乙腈含量对保留的影响曲线表明,这两种糖醇固定相具有典型的亲水作用色谱固定相性质,对极性和亲水性化合物有很强的保留作用。利用这两种固定相成功分离了水溶性维生素、水杨酸及其类似物、碱基及其相应的核苷和淫羊藿苷类似物等模型混合物,同时糖醇固定相展现了新颖的选择性,特别是相对于线形的木糖醇键合固定相,非线形的麦芽糖醇键合固定相表现出了对糖基的独特保留能力。此外,缓冲盐的pH和浓度对保留的影响表明静电作用在这两种糖醇固定相的保留机理中也发挥着一定的作用。本文所发展的糖醇类固定相具有良好的分离性能,有望在亲水作用色谱分离领域发挥潜在的应用价值。     

全自动固相萃取-高效液相色谱-串联质谱法测定食糖中的雌二醇

建立了全自动固相萃取-高效液相色谱-串联质谱检测食糖中雌二醇含量的方法。食糖样品经水溶解后,用碱化乙腈提取,经HLB固相萃取柱净化,采用高效液相色谱-串联质谱分析,内标法定量。质谱分析采用电喷雾电离(ESI)负离子扫描,多反应监测(MRM)模式。雌二醇定量离子对为271.1/144.8和271.1/183.2,内标D2-雌二醇定量离子对为273.2/147.0。实验表明,经SPE柱净化后基质效应明显降低,样品中添加0.5~10 μg/kg的雌二醇,其回收率为83.9%~95.1%,相对标准偏差(n=6)小于10%。雌二醇的检出限为0.1 μg/kg,定量限为0.5 μg/kg。该方法提取效果好,具有良好的灵敏度、回收率和重复性。     

Recent Advances in C5 and C6 Sugar Alcohol Synthesis by Hydrogenation of Monosaccharides and Cellulose Hydrolytic Hydrogenation over Non-Noble Metal Catalysts

A new reality of the 21st century is the transition to a new type of economy and energy concepts characterized by the replacement of existing petrochemical routes to a bio-based circular economy. The needs for new strategies in obtaining basic products from bio-based resources with minimum CO₂ traces has become mandatory. In this review, recent trends in the conversion of biomass-derived molecules, such as simple monomeric sugars and cellulose, to industrially important C₅ and C₆ sugar alcohols on heterogeneous catalysts based on non-noble metals are discussed focusing on the influence of catalyst structures and reaction conditions used on the substrate conversion and product selectivity. The challenges and prominent ideas are suggested for the further development of catalytic hydrogenation of naturally abundant carbohydrates to value-added chemicals on non-noble metal catalysts.     

Crystal Structure and Conformation of an 2-Amino-1,3-thiazine Derivative

Thiazine sugar derivative 2 was synthesized and characterized by IR, NMR and H RMS, and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system （C16H24N2O8S2, Mr = 436.49） with space group P21, a = 10.311（2）, b = 9.1198（18）, c = 11.623（2）A, β = 109.47（3）°, V= 1030.4（4）A^3, Z= 2, Dc = 1.407 g/cm^3, F（000）= 460, μ= 0.303 mm^-1, the final R = 0.0437 and wR = 0.0561 for 1954 observed reflections （I 〉 2σ（I））. Nine hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparison with the original material.