近红外漫反射光谱法快速测定秸秆青贮饲料成分含量

采用傅里叶近红外漫反射光谱技术,结合偏最小二乘回归法,以158个不同种类的秸秆青贮饲料样品建立了常规化学成分和发酵成分含量的近红外定量分析校正模型。其中常规化学成分中, 粗蛋白、中性洗涤纤维、酸性洗涤纤维、半纤维素、干物质、粗灰分和酸性洗涤木质素含量的校正模型决定系数R2分别为0.95,0.90,0.86,0.91,0.86,0.95和0.90;发酵成分的pH、乳酸、乙酸、丙酸、丁酸和氨态氮含量的校正模型决定系数R2分别为0.98,0.83,0.85,0.3,0.90和0.92。研究发现除乙酸、丙酸和丁酸之外,其他成分含量的相对分析误差RPD(SD/SECV)均大于2.5;除乳酸、乙酸、丙酸和丁酸之外,所建近红外定量分析模型对独立检验集样品其他成分含量的预测值与化学值的相关决定系数R2均大于0.08。该研究结果对青贮饲料品质的快速检测具有重要的实际意义。     

基于傅里叶红外光谱的癸酸-棕榈酸/SiO_2相变储湿复合材料制备机理研究

根据前期在相变储湿复合材料制备方面取得的成果,以SiO_2为载体材料、癸酸-棕榈酸为相变材料,采用溶胶-凝胶法制备癸酸-棕榈酸/SiO_2相变储湿复合材料。采用傅里叶红外光谱仪对癸酸-棕榈酸/SiO_2相变储湿复合材料制备过程各阶段的合成物质进行测试,即相变材料制备阶段、SiO_2载体材料制备阶段和癸酸-棕榈酸/SiO_2相变储湿复合材料制备阶段。研究SiO_2基相变储湿复合材料制备过程中SiO_2网络结构形成机理、癸酸-棕榈酸嵌入方式、癸酸-棕榈酸与SiO_2嵌合机理,阐明溶胶-凝胶法制备癸酸-棕榈酸/SiO_2相变储湿复合材料的相关机理。同时采用X射线衍射仪和扫描电子显微镜对癸酸-棕榈酸/SiO_2相变储湿复合材料的物质组成和微观形貌进行测试,以佐证癸酸-棕榈酸/SiO_2相变储湿复合材料的制备机理。结果表明:通过Si—O—Si基团断裂与重组形成大量闭合孔或笼有效地将癸酸-棕榈酸包覆,从而制备形成癸酸-棕榈酸/SiO_2相变储湿复合材料;在癸酸-棕榈酸/SiO_2相变储湿复合材料制备过程中癸酸-棕榈酸与SiO_2仅仅为物理嵌合,未发生任何化学反应;癸酸-棕榈酸/SiO_2相变储湿复合材料中SiO_2形成大量闭合孔或笼,一部分用于包覆癸酸-棕榈酸,发挥相变调温性能,另一部分利用其网络空隙结构,发挥储湿调湿性能,从而达到同时调节室内温度和湿度的目的。     

有机酸在电感耦合等离子体质谱中基体效应的研究

研究了乙二酸、乳酸、酒石酸和柠檬酸等有机试剂对不同质量和不同电离电位元素电感耦合等离子体质谱信号的影响。结果表明,随着雾化气流速的调节,低浓度有机酸介质对所分析元素具有增强效应,尤其是对电离电位在9～11 eV的Be,Zn,As,Se,Sb和Hg等高电离电位元素的影响。酒石酸的增强效应显著大于乙二酸、乳酸、柠檬酸。探讨了有机酸的增强机理。利用酒石酸对Be,Zn,As,Se,Sb和Hg等的增强特性,测定了水标准物质SRM 1640中的Be,Zn,As,Se,Sb和SRM 1641d中Hg,其测定结果与标准样品提供的标准值基本一致。     

Low-temperature transformations of orthoboric acid

The thermal transformations of orthoboric acid at 100–105°C in a vacuum (15 ± 5 torr) were studied. The conditions of the formation of β-metaboric acid were determined; β-metaboric acid is a promising product for the preparation of organo-inorganic incombustible polymeric materials with high thermal stability, fairly high hydrolytic stability, and satisfactory elastic properties. The metaboric acid polymorph formed in thermolysis substantially depended on the prehistory of the sample, primarily on microamounts of strongly bound water in orthoboric acid. Thermal treatment of a 1: 1 mixture of “dry” orthoboric acid and boric anhydride gave β-metaboric acid only, thermal treatment of dry orthoboric acid, a mixture of α- and β-metaboric acids, and heating of aqueous solutions of orthoboric acid gave α-metaboric acid only. During storage for three months even in a hermetically closed vessel, dry orthoboric acid absorbed moisture from air, and the products of its thermolysis did not contain β-metaboric acid. Water was absorbed reversibly, and, after thermal treatment of damp orthoboric acid at 60°C in a 10^?2 torr vacuum, the X-ray pattern of the product of its thermolysis again contained β-metaboric acid peaks. Note that α- and β-metaboric acids are unstable and transform back into orthoboric acid during storage.     

歧化松香中树脂酸异构体的NMR研究

树脂酸是松香的主要成分,歧化松香质量的好坏,主要取决于树脂酸的组分及其含量.本文测定了五种树脂酸——枞酸、新枞酸、左旋海松酸、长叶松酸和脱氢枞酸的¹H、¹³C、DEPT谱.并通过二维HMQC以及HMBC相关谱和模型化合物分别对其谱图的归属进行了详细的探讨.     

利用红外光谱分析有机羧酸在均相反应中的配位作用机理

利用红外(IR)光谱、X射线衍射(XRD)及透射电子显微镜(TEM)等手段,对有机羧酸在尿素及硝酸铈的均相反应混合溶液中所起的配位作用进行了分析,并对产品的物相和形貌进行了测试与表征。实验结果表明：在尿素及硝酸铈的混合溶液中分别加入一元羧酸硬脂酸,二元羧酸酒石酸和三元羧酸柠檬酸时,一元羧酸硬脂酸在混合溶液中只起表面活性剂的作用,其产物为斜方晶系的单晶Ce₂O(CO₃)₂·H₂O微粉,且表面活性剂硬脂酸的加入使得晶体的晶化程度明显提高;而二元羧酸酒石酸与三元羧酸柠檬酸在均相反应中则起螯合剂的作用,分别与Ce3+形成螯合物酒石酸铈和柠檬酸铈,这些结果的造成是由于其反应机理的不同所导致的。     

Preparation of biodegradable poly(lactic acid-co-aspartic acid) by copolymerization processes

Poly(lactic acid-co-aspartic acid) was obtained by copolymerizing DL-lactic acid and L-aspartic acid. The structure of poly(lactic acid-co-aspartic acid) was characterized by IR, ¹H NMR. The characters of poly(lactic acid-co-aspartic acid) were determined by hydrolytic degradable experiments, which indicate that the degradation rate of poly(lactic acid-co-aspartic acid) was accelerated by aspartic acid synthesized in the polymers.     

Study on the effect of different acids on the structure and photocatalytic activity of mesoporous titania

Nanocrystalline mesoporous titania was synthesized via a combined sol–gel process with surfactant-assisted templating method using cetyltrimethyl ammonium bromide (CTAB) as the structure-directing agent. The process was catalyzed by different acid (hydrochloric acid, nitric acid, sulfuric acid, or phosphoric acid). The prepared samples were characterized by XRD, TEM, BET and FT-IR. The photocatalytic activity of the samples was determined by degradation of phenol in aqueous solution. Results showed that different acid had different effect on the structure and crystal phase of the samples. The sample adjusted by phosphoric acid showed highest surface area and photocatalytic activity. The formation mechanism of the samples catalyzed by different acid was also discussed.     

猫爪草中的脂肪酸及有机酸的GC-MS分析

研究了用GC-MS法测定猫爪草中脂肪酸及有机酸的方法.河南产猫爪草块根粉碎后过20目筛,分别用石油醚(60～90℃)和乙醚回流提取6 h,提取液经浓缩后进行甲酯化,并由GC-MS法对其脂肪酸及有机酸的成分进行分析和鉴定.分析结果表明:两种提取剂的提取结果基本一致,猫爪草乙醚提取物中检测出含有23种物质,鉴定出其中的15种脂肪酸和有机酸,包括十四烷酸、十六烷酸、十八烷酸、二十烷酸、二十二烷酸、亚油酸、亚麻酸等,其中不饱和脂肪酸占58.19%,亚油酸占35.68%.     

农药丁吡吗啉与腐殖酸作用机理探讨

探讨农药丁吡吗啉与腐殖酸的作用机理, 可进一步了解农药在土壤中腐殖酸催化下降解的行为过程。将市售腐殖酸进行逐级分离,获得黄腐酸、棕腐酸和黑腐酸的固态或溶液状态,而后分别与农药丁吡吗啉进行作用,利用红外,荧光两种分析方法对其作用机理进行了解释。结果表明,三组分与丁吡吗啉之间广泛存在范德华力、次级键等弱作用力。黄腐酸与丁吡吗啉之间存在氢键和电荷转移吸附等作用力,棕腐酸与丁吡吗啉存在电荷转移吸附等作用力,黑腐酸与丁吡吗啉之间的作用力最弱,即依照黄腐酸、棕腐酸、黑腐酸三组分平均分子量依次递增的顺序,与农药丁吡吗啉之间的作用力依次降低。     

液相色谱法检测化妆品中3种防腐剂

建立了化妆品中防腐剂水杨酸、苯甲酸和山梨酸的高效液相色谱检测方法.试样经乙醇和硫酸处理后,由C18反相色谱柱进行分离,紫外检测器进行检测,用外标法定量.实验结果表明,该方法简便、高效,测定结果准确,适用于化妆品中水杨酸、苯甲酸和山梨酸含量的同时检测.     

Sonochemical effects on free phenolic acids under ultrasound treatment in a model system

Sonochemical effects on seven free phenolic acids under ultrasound treatment in a model system have been investigated. The degradation products have also been tentatively identified by FTIR and HPLC-UV-ESIMS. Five phenolic acids (protocatechuic acid, p-hydroxybenzoic acid, vanillic acid, p-coumaric acid, and ferulic acid) proved to be stable, while two others (caffeic acid and sinapic acid) were degraded under ultrasound treatment. The nature of the solvent and the temperature has been identified as important factors in determining the degradation reaction. Liquid height, ultrasonic intensity, and duty cycle of the ultrasound exposure affected only the degradation rate and did not change the nature of the degradation. The degradation rates of caffeic acid and sinapic acid decreased with increasing temperature. The degradation kinetics of these two acids under ultrasound conformed to zeroth-order reactions at ?5 to 25 °C. Both decomposition and polymerization reactions occurred when caffeic acid and sinapic acid were subjected to ultrasound. Degradation products, such as the corresponding decarboxylation products and their dimers, have been tentatively identified.     

吡啶羧酸在银电极表面随电极电位变化的表面增强拉曼光谱研究(英文)

本文通过表面增强拉曼散射研究了三种不同构型的吡啶羧酸—皮考酸、异烟酸和烟酸在粗糙银电极表面上的吸附形态随电极电位的变化关系。大量的表面结构信息可从丰富的表面拉曼信号及其随电极电位相应的变化而获得。分析表明在电极电位负移过程中皮考酸分子一直采取通过羧基和苯环上的N原子侧立吸附在银电极表面,与之不同的是,异烟酸分子和烟酸分子在表面的吸附状态都随电位改变发生了变化,我们对此进行了分析和解释     

系数倍率紫外光谱法同时测定复方苯甲酸软膏中的苯甲酸和水杨酸的研究

本文用系数倍率紫外光谱法同时测定了复方苯甲酸软膏中苯甲酸和水杨酸的含量,取得了满意的结果,苯甲酸测定回收率为99．33％－101．80％,水杨酸测定回收率100．92％－105．46％。     

铕-芳香羧酸-丙烯腈三元配合物的合成及发光性能研究

以对甲基苯甲酸、大茴香酸、间氯苯甲酸、苯甲酸和对羟基苯甲酸为第一配体,丙烯腈为反应型配体,合成了五种新的铕-芳香羧酸-丙烯腈三元配合物。通过元素分析,EDTA配位滴定分析,热分析,红外、紫外和荧光光谱分析对目标配合物的组成、结构进行了表征,并研究了它们的发光性能。结果表明,五种新的反应型铕三元配合物均具有良好的发光性能,各芳香羧酸向铕离子传递光能的能力为：对甲基苯甲酸＞苯甲酸＞间氯苯甲酸＞对羟基苯甲酸＞大茴香酸,将这些含反应型配体丙烯腈的发光铕配合物引入高分子化合物中可望合成出键合型铕高分子发光材料。     

Ultrasound-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum Ait

Oleanolic acid and ursolic acid are the main bioactive compounds in fruit of Ligustrum lucidum Ait, which possess anti-inflammatory, antioxidative, antiprotozoal, antimutagenic and anticancer properties. In this study, the ultrasound-assisted extraction of oleanolic acid and ursolic acid from L. lucidum Ait was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, extraction temperature and extraction time, on extraction efficiencies of oleanolic acid and ursolic acid from L. lucidum were evaluated. The influence of experimental parameters on extraction efficiency of ursolic acid was more significant than that of oleanolic acid. The optimal extraction conditions were 95% ethanol, the ratio of material to liquid at 1:20, and extraction for 10 min at 40 °C under ultrasonic irradiation. Under the optimal conditions, the yields of oleanolic acid and ursolic acid were 6.3 ± 0.25 and 9.8 ± 0.30 mg/g, respectively. The results indicated that the ultrasound-assisted extraction is a very useful method for the extraction of oleanolic acid and ursolic acid from L. lucidum.     

Application of MCR: Facile one-pot diastereoselective syntheses of novel chiral α,α'-iminodiacetic acid analogues

Several pairs of enantiomeric alpha,alpha'-iminodiacetic acid analogues (2 and 4) were prepared separately by highly diastereoselective 3CR, which involves a reaction of an isocyanide, an aldehyde, and an enantiomerically pure amino acid in methanol. Synthesis of each of the enantiomers was controlled by the configuration of the amino acid; L-amino acid produces one enantiomer and D-amino acid generates the other. The diastereoselectivity of the 3CR is very sensitive to the substituent size of both aldehyde and enantiomerically pure amino acid.     

显微红外光谱在摩擦学中的应用

用显微红外光谱测定了羟基植物油脂肪酸在摩擦过程中生成聚酯的特征吸收峰υc^as-o-c的波数，由聚酯的折合质量分析了特征吸收峰υc^as-o-c的波数位移，据此导出了羟基植物油脂肪酸的抗磨性顺序规律与振动吸收峰位置的内在联系，合理解释了υc^as-o-c从小到大的顺序（13，14－二羟基廿二酸＜13（14）－羟基廿二酸＝9，10－二羟基十八酸＜9，10，12－三羟基十八酯＜9（10）－羟基十八酸）与羟基酸的抗磨性从好到差的顺序（13，14－二羟基廿二酸＞13（14）－羟基廿二酸＝9，10－二羟基十八酸＞9，10，12－羟基十八酸＞9（10）－羟基十八酸）的一致性。13，14－二羟基廿二酸形成网状取酯膜，9（10）－羟基十八酸形成线状聚酯膜。     

基于拉曼成像技术的面粉中抗坏血酸添加剂定量检测研究

抗坏血酸是一种常见的面粉品质改良剂,用于改善面团的流变学特性及面包的烘焙品质。本研究以面粉中含不同浓度抗坏血酸的混合样品为研究对象,通过拉曼成像技术实现面粉中抗坏血酸的检测、识别和定量分析。分别采集面粉、抗坏血酸和面粉-抗坏血酸混合样品的拉曼图像,确定感兴趣区域及光谱范围,以抗坏血酸拉曼光谱中强度较高且区别于面粉的3处拉曼峰（631,1 128和1 658 cm-1）为依据对混合样品的平均拉曼光谱进行分析,结果显示其不能有效评估面粉中抗坏血酸含量,研究探索对图像中各像素点对应的拉曼光谱进行分析以实现面粉中抗坏血酸的有效检测。以混合样品图像中各像素点拉曼光谱作为校正集、面粉平均拉曼光谱和抗坏血酸平均拉曼光谱的线性组合光谱作为验证集建立偏最小二乘模型,模型的回归系数用于将混合样品的三维拉曼图像重建为二维灰度图像,通过阈值分割实现面粉中抗坏血酸的检测和识别,根据识别结果建立定量分析模型。结果显示,偏最小二乘模型的最高和最低回归系数分别对应于抗坏血酸和面粉的最强拉曼峰,所有回归系数应用于混合样品拉曼图像将其转换为灰度图像后面粉和抗坏血酸的像素点仍难以识别,阈值分割方法将灰度图像转换为用于分类面粉像素和抗坏血酸像素的二值图像实现了面粉中抗坏血酸的有效检测。通过分析各浓度混合样品对应子样品中识别到的抗坏血酸像素点数确定本研究对面粉中抗坏血酸的最低检测浓度为0.01%（100 mg·kg-1）,混合样品中抗坏血酸浓度同图像中识别到的抗坏血酸像素点在0.01%~0.20%范围内具有良好的线性关系,决定系数为0.996 0。研究结果可为面粉中抗坏血酸添加剂的定量检测提供方法支持,为大规模快速筛查提供了技术参考。     

Reference database of Raman spectra of biological molecules

Raman spectra of biological materials are very complex, because they consist of signals from all molecules present in cells. In order to obtain chemical information from these spectra, it is necessary to know the Raman patterns of the possible components of a cell. In this paper, we present a collection of Raman spectra of biomolecules that can serve as references for the interpretation of Raman spectra of biological materials. We included the most important components present in a cell: (1) DNA and RNA bases (adenine, cytosine, guanine, thymine and uracil), (2) amino acids (glycine, L ‐alanine, L ‐valine, L ‐serine, L ‐glutamic acid, L ‐arginine, L ‐phenylalanine, L ‐tyrosine, L ‐tryptophan, L ‐histidine, L ‐proline), (3) fatty acids and fats (lauric acid, myristic acid, palmitic acid, stearic acid, 12‐methyltetradecanoic acid, 13‐methylmyristic acid, 14‐methylpentadecanoic acid, 14‐methylhexadecanoic acid, 15‐methylpalmitic acid, oleic acid, vaccenic acid, glycerol, triolein, trilinolein, trilinolenin), (4) saccharides (β‐D ‐glucose, lactose, cellulose, D ‐(+)‐dextrose, D ‐(+)‐trehalose, amylose, amylopectine, D ‐(+)‐mannose, D ‐(+)‐fucose, D ‐(−)‐arabinose, D ‐(+)‐xylose, D ‐(−)‐fructose, D ‐(+)‐galactosamine, N‐acetyl‐D ‐glucosamine, chitin), (5) primary metabolites (citric acid, succinic acid, fumarate, malic acid, pyruvate, phosphoenolpyruvate, coenzyme A, acetyl coenzyme A, acetoacetate, D ‐fructose‐6‐phosphate) and (6) others (β‐carotene, ascorbic acid, riboflavin, glutathione). Examples of Raman spectra of bacteria and fungal spores are shown, together with band assignments to the reference products. Copyright © 2007 John Wiley & Sons, Ltd.