Chemical Characterization of Sorbitan Tri-Stearate Commercial Samples and Their Determination in Confectionery Fats by HPLC High-Resolution Mass Spectrometry

Nominal sorbitan tristearate (E492) commercial samples are widely used generally as emulsifiers and particularly as anti-bloom agents in confectionery products. In spite of this generalized use, their qualitative and quantitative evaluation is poorly documented in literature and the relative works go back to the last decades of last century. In the present work, a deep study by HPLC-High Resolution Mass Spectrometry of qualitative composition of five E492 commercial samples was made up showing a very complex pattern of stearic and palmitic acid esters with the sorbitol anhydrides, sorbitan, and isosorbide. A clear distinction of sorbitan mono-, di-, tri-, and tetra-esters, of sorbitol penta- and hexa-esters and isosorbide mono- and di-esters was achieved. Contemporarily, difference in the qualitative pattern between E492 commercial samples coming from different suppliers was established. As a consequence, quantitative evaluation can be reliably obtained by using as calibration standard the same E492 present in real samples. The accuracy and recovery of the method were determined allowing in this way a reliable application to commercial confectionery products. The detailed knowledge of STS composition may be of great help to orient the synthesis conditions in order to modulate its properties as a function of various experimental necessities.     

Composition,Structure, and Color of Fat Bloom Due to the Partial Liquefaction of Fat in Dark Chocolate

A type of fat bloom, which had not previously been fully characterized, was investigated to identify the state of its existence and its formation mechanism. Samples of bloom on solid chocolate resulting from the partial liquefaction of fat during temperature variations were analyzed to determine the crystal characteristics, fat contents, and triacylglycerol (TAG) compositions. Also, observation and elemental analyses were performed by scanning electron microscope with an energy-dispersive X-ray spectrometer, color analyses of minute regions were made by using PARISS^®, and Fourier-transform infrared (FT-IR) analyses were performed. The dark- and light-brown areas did not show any differences in fat content or TAG compositions that could lead to the observed color differences. Although differences in component distributions were noted in micrometer-sized regions, no relation to the colors was confirmed. The bloom samples in this study and bloom developed without a tempering process resembled each other in the tone of color at their discolored regions, but the states they adopted differed from one another. It is suggested that the color in this type of bloom was affected by the roughness and/or porosity of the microstructure and could also be a result of the coarsened fat crystal network and of the liquid fat migration.     

牦牛乳中DNA提取方法的建立与优化

为加速牦牛重要基因的挖掘和功能鉴定,以牦牛乳作为试验材料,建立简便的牦牛基因组DNA提取方法.采用常规离心法,从牦牛乳中获得体细胞,进而提取基因组DNA.研究不同去除蛋白方法、不同DNA沉淀剂、不同贮藏条件对牦牛乳中DNA提取质量的影响.DNA质量通过PCR评价.结果表明:高盐法与酚/氯仿法去除蛋白效果相当.高盐法简便...     

牦牛皮胶原蛋白的提取及其性能分析

以牦牛皮为原料,提取了酸溶性胶原蛋白(ASC)和酶溶性胶原蛋白(PSC),并对胶原蛋白分子的结构和性能进行了分析。结果表明:ASC和PSC的提取率分别为54%±0.18%和78%±0.42%;UV、FTIR及电泳分析结果表明:ASC和PSC具有完整的三股螺旋结构,符合Ⅰ型胶原蛋白的结构特征;氨基酸分析发现:ASC和PSC含有丰富的亚氨基酸,其含量分别为264.1和276.6残基/1000残基;热稳定性分析表明:ASC和PSC热变性温度(Td)分别为37.5、41.5℃,热收缩温度分别为62.5、70.0℃,证明PSC的热稳定性高于ASC;SEM结果表明:ASC和PSC表面为松散、不规则的纤维网形态;自组装实验结果显示:两者具有一定的成纤维能力,自组装产物的D-周期分别为(68.2±5)nm、(69.3±3)nm,且PSC比ASC的组装速度快。     

甘南拉卜楞寺酥油花艺术的数字化保护与思考

酥油花经国务院批准列入第一批国家级非物质文化遗产名录。本文以甘南夏河拉卜楞寺的酥油花艺术作品为例进行分析,希望通过借助现代数字手段有效地保护和传承藏族这门独有的文化艺术形式,让更多的人认识传统文化艺术的博大精深和保护非物质文化遗产的重要性,彰显文化自信。     

Thermal analysis of isothermal crystallization kinetics in blends of cocoa butter with milk fat or milk fat fractions

The kinetics of isothermal crystallization of binary mixtures of cocoa butter with milk fat and milk fat fractions were evaluated by applying the Avrami equation. Application of the Avrami equation to isothermal crystallization of the fats and the binary fat blends revealed different nucleation and growth mechanisms for the fats, based on the Avrami exponent. The suggested mechanism for cocoa butter crystallization was heterogeneous nucleation and spherulitic growth from sporadic nuclei. For milk fat, the mechanism was instantaneous heterogeneous nucleation followed by spherulitic growth. For milk fat fractions, the mechanism was high nucleation rate at the beginning of crystallization, which decreased with time, and plate-like growth. Addition of milk fat fractions did not cause a significant change in the suggested nucleation and growth mechanism of cocoa butter.     

Polymorphism and solidification kinetics of the binary system POS-SOS

As a first approach to modeling the crystallization behavior of cocoa butter, the binary system of its two major components, 1-palmitoyl-2-oleoyl-3-stearoyl-s n-glycerol (POS) and 1,3-distearoyl-2-oleoyl-s n-glycerol (SOS), was studied. Differential scanning calorimetry, coupled with polarized light microscopy, was used to determine the phase diagrams of the various polymorphic forms (the most metastable sub-α and α, intermediate δ and β′, and stable β). Associated theoretical phase diagrams were also built. The presence of a solid solution for β and the ideal behavior of α were confirmed. Kinetics of isothermal solidification as a function of temperature were studied for three compositions of the POS-SOS system. Results were displayed as time-temperature-transformation (TTT) diagrams and crystal morphology maps. Dependence of the crystallization kinetics on composition of the binary system was interpreted in terms of nucleation and growth mechanisms. The asymmetry of the POS molecule induces a slower growth rate of the mixture when the concentration of this triacylglycerol is increased. Solidification kinetics during continuous cooling were studied at various cooling rates for the system POS-SOS 25:75. Experimental results were compared with numerical predictions of a solidification model based upon TTT data and an additivity principle. The calculated and measured volume fractions of the different phases formed and times of onset and finish of the solidification were in good agreement.     

Identification of cocoa butter equivalents added to cocoa butter by fatty acid composition of the triacylglycerol sub-fractions separated by Ag+-HPLC – II –

 In a previous study the fatty acid compositions of triacylglycerol sub-fractions, separated by Ag⁺-HPLC, were studied in samples of cocoa butter, cocoa butter equivalents (CBE) and some of their mixtures. In this paper similar research is described which was carried out on three other CBE (Illexao 30–61, Illexao 30–63, Illexao 30–71). The results show the particular significance of the fully saturated sub-fraction, in which notable percentage changes in C16 : 0 and C18 : 0 contents were also detectable in the two mixtures with the lowest CBE content (5% or 15%, w/w) relative to genuine cocoa butter. Multiple regression analysis was used to verify the percentages changes of fatty acid contents in the fully saturated sub-fraction as a function of the percentage of CBE added to genuine cocoa butter. Received: 19 December 1997 / Revised version: 25 June 1998     

In-line measurement of tempered cocoa butter and chocolate by means of near-infrared spectroscopy

In the present work cocoa butter and chocolate were precrystallized by means of a newly developed shear crystallizer. The shear crystallizer was integrated into a circular loop. The handling of precrystallized cocoa butter showed a high dependency on the timing of applied analysis. Differential scanning calorimetry, calorimetry, rheometry, and in-line near-infrared (NIR) were all directly influenced by the fat crystal structure. Nevertheless, for cocoa butter it was shown that mechanical energy input (rpm) had a significant influence on viscosity, melting enthalpy, and slope at the second point of inflection of a temper curve. Experiments with cocoa butter at constant exit temperature showed a linear increase of viscosity between 0.1 and 0.8 Pa·s in the range of 300 to 1300 rpm. Melting enthalpy increased in the same rpm interval from 0.02 to 2.5 J/g. Solidification time (from 4.5 to 0.5 min) and slope (from 0.82 to 0.15, second point of inflection of temper curve) consequently decreased (both with exponential approximation). For cocoa butter, slope and solidification time correlated linearly whereas solidification time and viscosity followed a power law fit. This proved that defined relationships exist between rheological data and data from temper curve measurements. Viscosity was linearly dependent on crystal content. By means of NIR spectroscopy good correlation models for cocoa butter viscosity, enthalpy (crystal content), and slope values were found. For precrystallized chocolate, analytical values such as viscosity and slope values were detected off-line and used for calibration of NIR spectroscopy.     

Phase behavior and extended phase scheme of static cocoa butter investigated with real-time X-ray powder diffraction

A complete isothermal phase-transition scheme of cocoa butter under static conditions is presented, based on time-resolved X-ray powder diffraction experiments. In contrast to what is known from literature, not only β V, but also β VI can be obtained directly through transformation from β′. Another remarkable result is that β′ exists as a phase range rather than as two separate phases. Within this β′ phase range no isothermal phase transitions have been observed. More detailed information concerning the observed cocoa butter polymorphs was obtained by determination of melting ranges, using time-resolved X-ray powder diffraction. Also standard X-ray powder diffraction patterns of the γ, the α, and the two β phases and parts of the β′ phase range have been recorded. The observed phase behavior of cocoa butter has been explained based on the concept of individual crystallite phase behavior of cocoa butter