稻谷壳制备石墨烯纳米片及结构表征

为了充分利用南方丰富的稻谷壳资源,制备附加值较高的石墨烯纳米材料。该文采用稻谷壳可再生资源经高温炭化、过筛、透析等工艺等制备活性炭,将其在高纯氩保护下高温催化石墨化后制备的石墨微晶作为石墨烯的新型碳源。应用具有较大离子半径的硫酸根离子(0.295 nm)为插层剂预处理该石墨微晶,经水热及微波工艺制备石墨烯纳米片。采用透射电镜、扫描电镜、原子力显微镜、红外光谱、拉曼光谱及X射线衍射(X-ray diffraction spectroscopy,XRD)等技术对样品进行了形貌、结构和谱学等表征。原子力图表明,该石墨烯纳米片厚度范围为0.8~1.75 nm,为单层或双层石墨烯;由红外光谱可以观察到1 550 cm-1左右的石墨烯特征碳碳双键骨架振动峰。但未观察到传统Hummers氧化及水合肼法常出现,与石墨烯氧化后缺陷度有关的3 000~3 600 cm-1之间峰及1 250 cm-1左右振动峰。XRD数据显示所制备材料在24.7°亦具有石墨烯特征峰。拉曼光谱分析则显示,该方法所制备材料的与石墨烯层数相关的2D峰峰高接近G带的2倍,而与石墨烯缺陷度有关的D带峰峰高较小。该方法可成功制备单层或双层石墨烯纳米片,研究结果为高效制备基于稻谷壳可再生资源的石墨烯开辟了一条新路。     

Study of soybean seed coat components and their relationship to water absorption.

The occurrence of hard or "stone" seeds in shipments of food grade soybeans can cause serious problems in processing, particularly in the preparation of fermented soy products. Climatic conditions during the growing season and as the seed matures may trigger the production of hard seeds. Total water absorption of soybeans is also a significant parameter in assessing quality for export markets. The seed coats of six varieties of soybeans, covering a wide range of water absorption and stone seed content, were analyzed for ash and cations, protein, lignin, and complex carbohydrates. The water absorption characteristics and macrochemical constituents of the whole seed were also determined. The results indicated that there was no correlation between the concentration of any of the cations and the occurrence of hard seeds. The results from analysis of the complex carbohydrates indicated there were differences in hemicellulose content of seed coat fractions, particularly xylans, that correlated with the water uptake ratio and the occurrence of hard seeds.     

Preparation of plastic and biopolymer multilayer films by plasma source ion implantation

The plasma source ion implantation (PSII) technique was used to improve the adhesion between linear low-density polyethylene (LLDPE) and biopolymer. LLDPE was treated with the PSII using O(2) or CF(4) gas to modify its surface. After modification, chitosan or corn zein was used for coating on LLDPE. Wettability of the LLDPE surface was evaluated with a contact angle meter by the sessile drop method. X-ray photoelectron spectroscopy (XPS) was used to analyze the LLDPE surface. Before and after treatment, in the case of LLDPE treated with O(2) PSII, oxygen-containing functional groups were formed on the implanted surface. In the CF(4) PSII treated LLDPE, it was observed that the fluorine concentration on the surface of LLDPE remarkably increased and hydrophobic groups were formed by chemical reaction. Bilayer films coated with chitosan or corn zein showed 10 times lower oxygen permeability. Tensile strength of multilayer films was decreased a little compared with that of LLDPE. The plastic and biopolymer multilayer films have potential for food packaging application because of their O(2) gas barrier property and easy recyclability of the multilayer film.     

玉米粉制备生物质石墨烯与结构表征

针对目前石墨烯价格昂贵的缺点,该研究用高温炭化和氧化还原法以玉米粉为原料制备了生物质石墨烯.通过X射线光电子能谱对生物质石墨烯的组成元素进行分析,通过拉曼光谱、X射线衍射、原子力显微镜和透射电镜分析其结构和形貌.结果显示,生物质石墨烯的碳质量分数达95.1％;在衍射角为23.1°的(002)晶面处具有石墨烯的衍射峰,与...     

葡萄籽中水溶性钙结合蛋白的分离和鉴定

为了开发植物源葡萄籽补钙制剂,该研究通过亚细胞定位试验表明,葡萄籽的胚乳中含有大量的钙元素。通过电泳分析发现,葡萄籽的水溶性蛋白包括2种主要成分,其中一种是11 S球蛋白(蛋白质B),也是最主要的钙结合蛋白,另一种是表观分子量为670 k Da的蛋白质A。在蛋白质组成相同的情况下,用传统的碱溶酸沉法来分离葡萄籽蛋白会导致大量的钙流失。但用30%~50%硫酸铵沉淀法得到的蛋白质得率是(22.5±0.02)g/kg,蛋白质中钙质量分数(3.47%)是碱溶酸沉法(1.11%)的3倍。该研究结果为食品工业中矿物结合蛋白质的分离纯化提供参考。     

11S and 7S globulins of coconut (Cocos nucifera L.): purification and characterization

Total globulins extracted with 0.4 M NaCl in buffer from coconut endosperm separated into two peaks on gel filtration: peak I corresponding to 11S globulin or cocosin and peak II to 7S globulin with native molecular weights of 326 000 and 156 000, respectively. The percent composition of total globulins was estimated to be 11S, 86% and 7S, 14%. On SDS-PAGE, cocosin resolved into two closely migrating bands at approximately 34 000 (acidic polypeptide) and another set of 2 bands at 24 000 (basic polypeptide). Each set consisted of one darkly stained band and one lightly stained band. The 7S globulin consisted of three bands of 16 000, 22 000, and 24 000. Three isoforms of cocosin were identified after anion exchange chromatography. Cocosin, but not the 7S, was found to have disulfide bonds. Using periodic acid-Schiff's reagent, all of the bands of cocosin on SDS-PAGE were positive for carbohydrate. However, when con A-peroxidase was used, only the basic polypeptide stained positively for carbohydrate. For the 7S globulin, no carbohydrate group was detected using the PAS and con A-peroxidase tests. The 7S globulin was easily extracted with 0.10-0.15 M NaCl, whereas cocosin was extracted with 0.35 M NaCl. The N-terminal amino acid sequences of the 34 k band and 24 k band of cocosin were SVRSVNEFRXE and GLEETQ, respectively, and that of the 7S was EQEDPELQK.     

大豆磷酸烯醇式丙酮酸磷酸酯酶(PEPP)研究: Ⅱ.纯化与特性

从大豆叶片中分离磷酸烯醇式丙酮酸磷酸酯酶（phosphoenolpyruvate phosphatase，PEPP），通过硫酸胺分部（20％～50％饱和度）沉淀、DEAE-纤维素层析、羟基磷灰石层析将酶纯化了96．81倍，酶活性达17．91U／mg蛋白。该酶专一性较强，米氏常数（Km）为0．39mmol／L（PEP），最适pH6．8，在PH6．O～7．4范围内及50。C以下较稳定，被Mg^2＋、Mn^2＋激活，F^-、Cu^2＋、Zn^2＋、PO^3-、MoO4^2-抑制。     

Preparation and characterization of beta-carotene nanodispersions prepared by solvent displacement technique

This work demonstrated the preparation of protein-stabilized beta-carotene nanodispersions using the solvent displacement technique. The emulsifying performance of sodium caseinate (SC), whey protein concentrate (WPC), whey protein isolate (WPI), and a whey protein hydrolysate (WPH, 18% degree of hydrolysis) was compared in terms of particle size and zeta-potential of the nanodispersions. SC-stabilized nanodispersions exhibited a bimodal particle size distribution: large particles (stabilized by casein micelles) with a mean particle size of 171 nm and small particles (stabilized by casein submicelles) of 13 nm. This was confirmed with transmission electron microscopy analysis. Most of the beta-carotene precipitated (87.6%) was stabilized in the small particles. On the other hand, the nanodispersions stabilized by the whey proteins were polydispersed with larger mean particle sizes. The mean particle size of WPC and WPI was 1730 and 201 nm, respectively. The SC-stabilized nanodispersion was expected to be more stable as indicated by its higher absolute zeta-potential value (-31 mV) compared to that of WPC (-15 mV) and WPI (-16 mV). Partially hydrolyzed whey protein possessed improved emulsifying properties as shown by WPH-stabilized samples. It was interesting to note that increasing the SC concentration from 0.05 to 0.5 wt % increased the particle size of beta-carotene stabilized by casein micelles, while the reverse was true for those stabilized by SC submicelles. Microfluidization at 100 MPa of SC solution dissociated the casein micelles, resulting in a decrease in mean particle size of the casein micelle-stabilized particles when the SC solution was used to prepare nanodispersions. The results from this work showed that protein-stabilized beta-carotene nanodispersions could be prepared using the solvent displacement technique.     

Analysis of bromide ion in wine by ion selective electrode.

The use of the bromide ion selective electrode for the determination of bromide ion in wine has been found to be rapid and reliable. The method has been used for still wines and carbonated wines and is applicable to all wines regardless of their country of origin. The method consists of treating a 50 ml aliquot of wine with 2 ml each of 3.75M H3PO4, saturated KNO3, and 1M CuSO4. After 10 min the electrodes are immersed in the samples and a millivolt reading is obtained. One hundred mul 500 ppm bromide ion standard is added and the millivolt reading is taken. Bromide ion concentration in the wine equals (Cdelta x 1)/((antilog deltaE/S)-1) where Cdelta equals 1, deltaE equals the change in potential expressed in millivolts, and S equals the electrode slope.     

Isolation and characterization of endophytic bacteria from wild and cultivated soybean varieties

Endophytic bacteria were isolated from surface sterilized stems, root, and nodules of wild and cultivated soybean varieties. Various phenotypic traits that are expected to be involved in the persistence and functions of the bacteria were analyzed. Most of the isolates from soybean were motile and indoleacetic acid producers, and 70 and 33% of isolates excreted cellulase and pectinase, respectively. These traits may be involved in endophytic characteristics in soybean. Some isolates were resistant to Str₁₀₀, formed capsules, and produced fluorescent pigments. Molecular characterization of selected 35 endophytic bacteria by 16S rDNA–polymerase chain reaction–restriction fragment length polymorphism showed two main clusters at 48 and 43% similarity coefficients in which most of the endophytes belonged. The genetic variation was more among endophytes isolated from Glycine max tissues than from G. soja.     

Diversity of seed globulins in Lathyrus sativus L. and some related species

Sodium dodecyl sulphate-polyacrylamide gel electrophoresis of reduced seed globulins covered 141 accessions of Lathyrus sativus and the following related species: L. amphicarpos, L. blepharicarpus, L. cicera, L. gorgoni, L. marmoratus, L. pseudocicera and L. stenophyllus. In the total examined material 71 globulin polypeptide bands were distinguished. The number of polypeptide bands detected in particular species varied from 14 in L. amphicarpos to 29 in L. sativus; all the species under study showed intraspecific variation due to individual variation and/or differences among accessions. Electrophoretic data were subjected to statistical analysis using hierarchical UPGMA grouping. Frequency distribution of polypeptide bands in L. sativus showed some correlations with geographical origin and certain seed characteristics (seed coat colour, seed weight) of the studied accessions. As regards interspecific relationships, the studied species showed to be distantly related taxa except for the rather closely allied L. cicera and L. marmoratus. The obtained results are compared with the electrophoretic seed albumin data reported earlier for the same taxa.     

Preparation of stable isotope-labeled 2-nitrobenzaldehyde derivatives of four metabolites of nitrofuran antibiotics and their comprehensive characterization by UV, MS, and NMR techniques

A convenient method is presented for the preparation of the carbon-13-labeled 2-nitrobenzaldehyde derivatives of the nitrofuran metabolites 3-amino-2-oxazolidinone (AOZ), semicarbazide (SC), 1-aminohydantoin (AH), and 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ), with the purpose of using them as internal standards for the quantification of trace levels of nitrofuran residues by liquid chromatography-tandem mass spectrometry in foods of animal origin. The synthesis encompasses the nitration of [1,2,3,4,5,6-(13)C(6)]toluene prior to chromyl compound-mediated oxidation of the methyl group into the corresponding aldehyde. The four metabolites of nitrofuran antibiotics were derivatized independently with the resulting ring-labeled 2-nitrobenzaldehyde (NBA) to obtain the target compounds. Both the isotopically enriched and native substances were used to perform a comprehensive fragmentation study by electrospray ionization (ESI) collision-induced dissociation (CID) mass spectrometry (MS). Full characterization of the nitrofuran derivatives was accomplished with ultraviolet (UV) and exhaustive nuclear magnetic resonance (NMR) analysis. A major advantage of the described procedure is that it can be extended to the preparation of other carbon-13-labeled derivatives of metabolites of nitrofuran antibiotics.     

可生物降解树脂包膜尿素的研制及性能

以聚碳酸亚丙酯（PPC）与聚丁二酸丁二醇酯（PBS）两种可生物降解树脂作为包膜材料,研制不同PPC/PBS组方包膜溶液,铺膜后初步确定两种材料混合的最佳比例;采用流化喷涂分别制备包膜尿素。通过分光光度法研究不同肥料的初期溶出率,采用扫描电镜观察包膜结构。结果表明,PPC与PBS的质量比在7∶5时,材料之间融合较好,质地较柔软,适合作为肥料包膜材料。实验证明此包膜材料在尿素表面能够形成细腻光滑致密的膜,可以适应尿素颗粒表面的外形轮廓而将其紧密覆盖。尿素包膜后,对尿素氮的释放有明显的控释作用,且在一定范围内,减少包膜所用时间或增加树脂用量都能增强控释效果。     

热塑性微细化淀粉的制备及其结构性能研究

为提高淀粉的热塑性能，优化其加工工艺，以超音速气流粉碎机制备微细化淀粉，确定微细化淀粉的最佳塑化条件，并利用扫描电镜、力学测试和示差扫描量热仪表征热塑性微细化淀粉。结果表明，微细化淀粉的热塑化最佳条件为：丙三醇与聚乙烯醇体积比为5∶1，微细化淀粉含量80%，共混温度160℃，单螺杆转速40 r/min。热塑性微细化淀粉呈现均匀的微观形貌，其拉伸强度为17.36 MPa，断裂伸长率138.29%，于130～155℃温度下熔融，加工性能良好。     

Preparation of whey protein hydrolysates using a single- and two-stage enzymatic membrane reactor and their immunological and antioxidant properties: characterization by multivariate data analysis

An initial 5% (w/v), followed thereafter with replacement aliquots of 3% (w/v), whey protein isolate (WPI) (ca. 86.98% Kjeldahl N x 6.38), was hydrolyzed using Protease N Amano G (IUB 3.4.24.28, Bacillus subtilis) in an enzymatic membrane reactor (EMR) fitted with either a 10 or 3 kDa nominal molecular weight cutoff (NMWCO) tangential flow filter (TFF) membrane. The hydrolysates were desalted by adsorption onto a styrene-based macroporous adsorption resin (MAR) and washed with deionized water to remove the alkali, and the peptides were desorbed with 25, 50, and 95% (v/v) ethyl alcohol. The desalted hydrolysates were analyzed for antibody binding, free radical scavenging, and molecular mass analysis as well as total and free amino acids (FAA). For the first time a quantity called IC50, the concentration of peptides causing 50% inhibition of the available antibody, is introduced to quantify inhibition enzyme-linked immunosorbent assay (ELISA) properties. Principal component analysis (PCA) was used for data reduction. The hydrolysate molecular mass provided the most prominent influence (PC1 = 57.35%), followed by inhibition ELISA (PC2 = 18.90%) and the antioxidant properties (PC3 = 10.43%). Ash was significantly reduced in the desalted fractions; the protein adsorption recoveries were high, whereas desorption with alcohol was prominently influenced by the hydrophobic/ hydrophilic amino acid balance. After hydrolysis, some hydrolysates showed increased ELISA reactivity compared with the native WPI.     

炭活化一步法制备豆渣基极微孔活性炭

鉴于以含氮生物质为原料,采用炭化碱活化两步法制备掺氮活性炭的工艺较长,该研究以大豆渣为原料,K2CO3为活化剂,尝试采用炭活化一步法制备含极微孔的掺氮活性炭,并考察活化温度对活性炭化学组成、孔结构及低压CO2吸附性能的影响。研究表明,该方法可用于制备富含极微孔的掺氮活性炭。当活化温度从560℃升高到650℃时,1)活性炭的氮元素皆均匀分布在体相及表面,其质量分数(4.1%~4.4%)变化不大,而其化学状态发生变化;2)比表面积、总孔容、微孔孔容均呈单调递增,但极微孔孔容先增大后减小。活化温度为600℃的样品,极微孔孔容较大(0.13 m L/g),极微孔主要集中在0.42~0.70 nm,微孔孔容、总孔容、比表面积分别为0.40 m L/g、0.43 m L/g、948 m2/g。该样品在10 k Pa、0℃下的CO2吸附量达1.94 mmol/g,CO2/N2表观选择性为41.6,说明它对低压CO2能同时展现出较高的吸附量及表观选择性。该研究为含氮活性炭的便捷制备提供了参考。