Fabrication and characterization of cellulose nanoparticles from maize stalk pith via ultrasonic-mediated cationic etherification

In this study, parenchyma cellulose, which was extracted from maize stalk pith as an abundant source of agricultural residues, was applied for preparing cellulose nanoparticles (CNPs) via an ultrasound-assisted etherification and a subsequent sonication process. The ultrasonic-assisted treatment greatly improved the modification of the pith cellulose with glycidyltrimethylammonium chloride, leading to a partial increase in the dissolubility of the as-obtained product and thus disintegration of sheet-like cellulose into nanoparticles. While the formation of CNPs by ultrasonication was largely dependent on the cellulose consistency in the cationic-modified system. Under the condition of 25% cellulose consistency, the longer sono-treated duration yielded a more stable and dispersible suspension of CNP due to its higher zeta potential. Degree of substitution and FT-IR analyses indicated that quaternary ammonium salts were grafted onto hydroxyl groups of cellulose chain. SEM and TEM images exhibited the CNP to have spherical morphology with an average dimeter from 15 to 55 nm. XRD investigation revealed that CNPs consisted mainly of a crystalline cellulose Ι structure, and they had a lower crystallinity than the starting cellulose. Moreover, thermogravimetric results illustrated the thermal resistance of the CNPs was lower than the pith cellulose. The optimal CNP with highly cationic charges, good stability and acceptable thermostability might be considered as one of the alternatively renewable reinforcement additives for nanocomposite production.     

Lecithin/propanol-based microemulsions used as media for a cholesterol oxidase-catalyzed reaction

Reverse micelles, Winsor III and IV systems were examined as reaction media for the enzymatic conversion of cholesterol to cholestenone by cholesterol oxidase at 298.2 K. The micelles and the microemulsions, stabilized by soybean lecithin and ethanol or 1-propanol as cosolvent, were characterized with respect to phase behavior and distribution of 1-propanol between the phases of the Winsor III systems. The used oils were dodecane, tetradecane, and hexadecane. The Winsor IV systems and the surfactant-rich phase in the Winsor III systems exhibit bicontinuous structures. The reaction yield for the enzymatic conversion performed in a Winsor IV system was much higher than in a Winsor III system or in reverse micelles.     

Determination of the residue of quizalofop-p-tefuryl in soybean by HPLC

A HPLC method was developed for the analysis of quizalofop-P-tefurylof in soybean. The samples were extracted with methanol-water (volume ratio), The extracts were cleaned up with a column of silica gel. The final residue was detected by HPLC, using a UV detector. The recoveries from the analytical method for soybean were 84.32%–89.25%. Variable coefficients were 0.49%∼1.51%. This method proved to be simple, reliable and accurate. __________ Translated from Chinese Journal of Chromatography, 2005, 23(2)(in Chinese)     

Stereoselectivity and competing reactions as studied by lipase-catalyzed esterifications in aqueous lecithin-based gelatin gels

 The enzyme catalyzed conversion of R/S-(±)-2-octanol with hexanoic acid to R/S-(±)-2-octyl hexanoate has been studied in different microenvironments and in the presence of the competing substrate ethanol. The reactions were performed in various gels made from aqueous gelatin solutions and liposome dispersions or isotropic liquid solutions, with or without oil and ethanol. The lipase Candida sp. (SP 525) was dissolved in the dispersions or solutions stabilized by the naturally occurring zwitterionic surfactant soybean lecithin. The sectioned porous gel was immersed in hexane containing 0.33 mol dm^-3 of racemic 2-octanol and hexanoic acid. Since ethanol acts both as a substrate and as a part of the gel it is of fundamental interest to know the phase behaviour of the used systems. Partial phase diagrams for the systems ethanol–water–soybean lecithin and ethanol/water (7:3)–oil–soybean lecithin were determined at 298.2 K. The oil was either castor oil or hexadecane. The conversion of R-2-octyl hexanoate was about 0.45 when no or small amounts of ethanol was present, but decreased considerably with high amounts of ethanol present and ethyl hexanoate became the main product. Hydrolysis of R-2-octyl hexanoate was favoured in the latter systems and hexanoic acid formed was immediately esterified to ethyl hexanoate. The conversion of R-2-octyl hexanoate and ethyl hexanoate depends only on the ethanol content present in the systems and is thus independent of the environment of the enzyme. However, the chiral esters synthesized from racemic 2-octanol and hexanoic acid showed high optical purities regardless of the ethanol content. Received: 1 July 1996 Accepted: 30 August 1996     

Development of a bionematicide with Paecilomyces lilacinus to control Meloidogyne incognita

Root-knot disease caused by Meloidogyne incognita is a matter of grave concern because it affects several economically important crop plants. The use of solid-state fermentation (SSF) may help to elaborate efficient formulations with fungi to be employed in the biologic control of nematodes. Attempts were made to select low-cost substrates for spore production of a strain of Paecilomyces lilacinus with known nematicide capacity. Coffee husks, cassava bagasse, and defatted soybean cake were utilized as substrates, and sugarcane bagasse was used as support. Fermentations were carried out in flasks covered with filter paper at 28°C for 10 d. The products obtained by SSF were evaluated for their nematicide activity in pot experiments containing one seedling of the plant Coleus inoculated with the nematode M. incognita. The plants were evaluated 2 mo after inoculation. Fermented products showed a reduction in the number of nematodes. The best results were obtained with defatted soybean cake, which showed almost 100% reduction in the number of nematodes; the reduction with coffee husk was 80% and with cassava bagasse was about 60%.     

Multivariate monitoring of soybean oil ethanolysis by FTIR

In this work, an analytical procedure was developed to monitor the ethanolysis of degummed soybean oil (DSO) using Fourier-transformed mid-infrared spectroscopy (FTIR) and methods of multivariate analysis such as principal component analysis (PCA) and partial least squares regression (PLS). The triglycerides (reagents) and ethyl esters (products) involved in ethanolysis were shown to have similar FTIR spectra. However, when the FTIR spectra derived from seven standard mixtures of triolein and ethyl oleate were treated by PCA at the region that represents the CO stretching vibration of ester groups (1700-1800 cm⁻¹), only two principal components (PC) were shown to capture 99.95% of the total spectral variance (92.37% for the former and 7.58% for the latter PC). This observation supported the development of a multivariate calibration model that was based on the PLS regression of the FTIR data. The prevision capability of this model was measured against 40 reaction aliquots whose ester content was previously determined by size exclusion chromatography. Only small discrepancies were observed when the two experimental data sets were treated by linear regression (R²=0.9837) and these deviations were attributed to the occurrence of non-modeled transient species in the reaction mixture (reaction intermediates), particularly at short reaction times. Therefore, the FTIR/PLS model was shown to be a fast and accurate method to predict reaction yields and to follow the in situ kinetics of soybean oil ethanolysis.     

Adventages and limits on usage of thermal methods in complex systems

In order to increase the nutrition value of bread, one of the most commonly used foodstuff all over the world, different additives are used in bread processing. In this paper we describe the thermal changes in bread and that of with 0.5% crude soybean lecithin additive. Their thermal stability has been investigated by TG, DSC and EGD methods. The thermal changes were also followed of soy products, lecithin and lysine, ingredients used as bread additives in order to check if they may suffer any thermal degradation during the baking process. The data obtained can be of use only for qualitative conclusions. According to the obtained data at the usual bread baking temperature only the additives in crust may partly decompose while in the crumb, at lower temperatures the additives, due to baking, are not damaged. The thermal methods give a possibility for rapid estimation of processes induced by heat effects in additives during the baking, and they are suitable to detect the changes during the bread-making procedure. However, they are neither suitable to provide any quantitative data on these changes nor facts affecting the nutrition value and of the bread.     

大豆油煎炸过程理化指标与LF-NMR弛豫特性的相关性研究

在对大豆油无料/薯条煎炸过程[温度:(180±5)℃,持续36 h]中的酸价(AV)、粘度(V)、吸光值(A)及总极性化合物(TPC)含量等及低场核磁共振(LF-NMR)弛豫特性(峰起始时间T21、T22、T23、相应的峰面积比例S21、S22、S23、单组份弛豫时间T2W)变化规律研究的基础上,利用多元回归分析建立了理化指标与其LF-NMR检测结果的相关性模型,并进行验证。结果表明:大豆油的酸价、TPC含量及S21峰面积均随煎炸时间的延长而线性增大,T21、T22峰起始时间及T2W则随煎炸时间的延长而线性减小(r2>0.90),粘度、吸光值随煎炸时间的延长逐渐增加并符合二项式关系(r2>0.90),而T23峰起始时间及S22、S23与煎炸时间之间无明显规律性变化。煎炸薯条后,油样的酸价、粘度、TPC含量、吸光值及S21均较无料煎炸显著增大(P<0.05),而T21、T22峰起始时间及T2W显著缩短。多元回归分析表明,酸价及TPC含量与T2W、T21,粘度与T2W,吸光值与S21间均可建立良好的相关性模型(R2>0.93)。模型验证合理可靠,可通过油样的LF-NMR检测结果有效预测其理化指标的变化。     

豆腐生产过程中微量元素硒分布特性研究

为确定以不同硒含量的大豆为原料生产豆腐过程中硒分布特性,用石墨炉原子吸收分光光度法对该过程中各种产物的硒含量进行了分析研究。结果表明,以硒含量分别为0.692、2.561、2.801 mg/kg的大豆为原料生产得到的豆腐、黄浆水、豆渣的硒含量分别为:0.089、0.250、0.138 mg/kg,0.462、0.760、0.507 mg/kg和0.532、0.764、0.524 mg/kg。豆腐生产过程中,以低硒大豆为原料生产豆腐,硒总回收率为75.59%;采用富硒大豆为原料生产,硒的回收率分别达到87.37%、87.20%;生产过程中豆腐、黄浆水和豆渣中硒含量占总回收硒的比率分别为39.01%～49.97%、23.92%～29.89%、26.11%～30.92%。     

流动注射化学发光法测定大豆异黄酮

基于在NaOH碱性介质中,K3Fe(CN)6可以直接氧化大豆异黄酮产生强的化学发光这一现象,并结合流动注射分析技术,提出了直接化学发光测定大豆异黄酮含量的新方法。当K3Fe(CN)6浓度为5.0×10-4mol/L,NaOH浓度为0.5 mol/L,主副蠕动泵转数分别为45 r/m in和35 r/m in时,体系具有最强的化学发光。该方法测定大豆异黄酮的线性范围为1.0×10-3~0.5 g/L;其回归方程为A(峰面积)=193305C(mg/L) 229.97,r=0.9962;检出限为4.6×10-4g/L。对5.0×10-3g/L大豆异黄酮溶液连续测定,每次得3个峰值,重复7次,相对标准偏差为2.46%。本方法已用于大豆中异黄酮含量的测定。