An activated-state model for the prediction of solid-phase crystallization growth kinetics in dried lactose particles

Molecular-level understanding of solid-phase crystallization growth kinetics has the potential to improve the fundamental basis for understanding this process. This understanding has been developed here as part of an activated-state model, which accounts for the effects of the moisture content and the temperature on the crystallization rate. Water-induced crystallization (WIC) at different temperatures (15 °C, 25 °C, 40 °C) and a constant relative humidity (75%) environment has been used to analyze the changes in enthalpy, entropy and Gibbs free energy of activation for the solid-phase crystallization of lactose. WIC showed that, at higher temperatures, crystallization commences at lower moisture contents. The enthalpy and Gibbs free energy of activation increased during the crystallization process, which suggested that the binding energy needed for the formation of an activated complex increased as the moisture content decreased, making the formation of the activated complex more difficult. The entropy of activation, on the other hand, decreased with the decrease in the moisture content. From the activated rate equation, the energy of activation has been estimated to be 39 ± 2 kJ mol⁻¹, which is similar to the literature value (40 kJ mol⁻¹) for the solid-phase crystallization of lactose. The reaction rate constant at 25 °C is 1.4 × 10⁻⁴ s⁻¹, which is similar to the literature value of 1.3 × 10⁻⁴ s⁻¹. The WLF equation is inconsistent and hence unreliable in predicting the rates of crystallization at the glass-transition temperature from the analysis of experimental data at different temperatures.     

Growth kinetics of WC-Fe layer formed at the surface iron during solid-phase diffusion

Tungsten carbide-reinforced iron-based surface composites were prepared via in situ solid-phase diffusion method; the variables included three temperatures (1085, 1100, and 1125 °C) and four heat treatment times (15, 45, 75, and 105 min). The samples were examined by X-ray diffraction, scanning electron microscopy, and Vickers hardness test. Results show that the tungsten carbide-reinforced iron-based surface composites consist of WC, α-Fe, W, and iron carbide phases, and the thickness of the WC-Fe layer ranges from 20.57±1.24 µm to 63.27±2.02 µm at 1085 °C. Furthermore, the maximum microhardness value of the WC-Fe layer at 1085 °C for 15 min is 2169 HV_0.1, whereas that of the iron matrix is 239 HV_0.1; such values demonstrate that the hardness of the composites are markedly enhanced. The kinetic of WC-Fe layer was analyzed by measuring the depth of pure WC layer as a function of heat treatment time and temperature. The results show a parabolic relationship between the thickness of pure WC layer and heat treatment time, and the activation energy for the pure WC layer was estimated to be 184.06 kJ mol⁻¹.     

预硫化加氢催化剂钝化技术研究进展

钝化是预硫化加氢催化剂的关键处理过程。预硫化催化剂经过钝化处理后,有效抑制了自热性质和硫的脱离,便于催化剂的存储和运输,并保持催化剂的活性,有利于器外预硫化催化剂的大规模生产。介绍了气相、液相和固相3种钝化方式、钝化机理及其应用和研究进展。     

Furan in the baby-food samples purchased from the Finnish markets – Determination with SPME–GC–MS

A method applying solid-phase microextraction followed by gas chromatography–mass spectrometric determination was in-house validated and used to study furan concentrations in baby-food samples purchased from the Finnish markets. The validation parameters showed that the method was well applicable for the reliable analysis of furan. Furan was analysed in 21 different baby-food samples as three independent replicates. The mean levels of furan varied between 4.7 and 90.3 μg kg⁻¹ being well in accordance with the levels reported in other studies. The mean concentrations of similar product formulas based on their ingredients were 9.2, 37.0 and 49.6 μg kg⁻¹ for fruit-, vegetables- and meat-containing baby-foods, respectively. According to the statistical analyses, fruit-based baby-food samples had significantly lower concentrations of furan as compared to other formulas. Based on our exercise, it seems that a low margin of safety exists between the extreme worst case infant exposures and the deduced NOAEL of furan on experimental animals, particularly for a clear rodent carcinogen.     

Profiling of volatile compounds of Phyllostachys pubescens shoots in Taiwan

This study examined the influence of heating temperature and duration on volatile aromatic components of spring and winter Phyllostachys pubescens shoots using SPME. Results from GC–MS analyses revealed that the main constituents in both bamboo shoots at ambient temperature include methoxy-phenyl oxime, followed by n-hexanol and 3Z-hexenal, which gives a fresh green aroma. Comparing the different compounds, between spring and winter shoots, revealed that spring bamboo shoots at ambient temperature comprise 12.30% methyl salicylate, which provides protection against insect attack, and 9.71% epi-cedrol; while winter bamboo shoots comprise 17.00% 1-octen-3-ol, which produces a distinct mushroom aroma. After heating at 100 °C for 60 min, a marked increase in relative content of benzyl salicylate (43.30%) and a significant decrease in methyl salicylate content in spring bamboo shoots were observed; while the major compound in winter bamboo shoots was n-heneicosane (78.09%) and the content of specific 1-octen-3-ol significantly decreased.     

Aroma profiles of five basil (Ocimum basilicum L.) cultivars grown under conventional and organic conditions

A headspace solid-phase microextraction (HS-SPME) method coupled to gas chromatography–ion trap mass spectrometry (GC–ITMS) has been developed and applied for profiling of volatile compounds released from five Ocimum basilicum L. cultivars grown under both organic and conventional conditions. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC–TOFMS) was employed for confirmation of identity of volatiles extracted from the basil headspace by SPME.     

Effects of ageing and low internal temperature of grilling on the formation of heterocyclic amines in beef Longissimus dorsi muscle

The mutagenic heterocyclic amines (HAs) originate in processed proteinaceous food. The effects of ageing (non-aged - i.e. 24 h post mortem vs. 14 and 28 days post mortem kept at 1 °C) and final internal temperature on cooking (T_i, 65 and 80 °C) on the content of HAs in grilled steaks (two-plated grill, temperature of 220 °C) were studied. HA precursors (creatine, creatinine, and free amino acids) and ageing indicators, such as instrumentally measured colour values, pH_ultimate values and length of myofibrilar fragments on raw and cutting values on grilled beef Longissimus dorsi muscles were determined. The muscles originated from eight commercially slaughtered Simmental bulls, 19-20 months old. The content of HAs was determined by a solid-phase extraction procedure. Meat ageing is accompanied by large changes in the chemical composition and structure of muscle tissues. In general, all the ageing indicators and precursors of HAs were influenced by ageing time at the 5% level or less. Creatine content declined significantly (non-aged: 6.00 mg g⁻¹, 14 days: 5.82 mg g⁻¹, and 28 days: 5.55 mg g⁻¹) and creatinine increased with days of ageing (non-aged: 0.19 mg g⁻¹, 14 days: 0.24 mg g⁻¹, and 28 days: 0.26 mg g⁻¹). Higher contents of total free amino acids were determined after 14 and 28 days of storage (28.18 μmol g⁻¹ and 37.59 μmol g⁻¹) than in non-aged beef (19.00 μmol g⁻¹). In this study, two HAs were determined: MeIQx (2-amino-3,8-dimethyl-imidazo[4,5-f]quinoxaline) and PhIP (2—amino-1-methyl-6-phenylimidazo-[4,5-b]pyridine). The content of HAs increases with ageing. At lower T_i, more MeIQx was formed; at higher T_i, more PhIP was formed. MeIQx was present in all samples while PhIP was found only in samples grilled to higher T_i. Samples treated to T_i = 80 °C generally contained less HAs (non-aged meat: 0.20 ng g⁻¹, 14 days: 0.26 ng g⁻¹, and 28 days: 0.28 ng g⁻¹) than samples treated to T_i = 65 °C (non-aged meat: 0.19 ng g⁻¹, 14 days: 0.36 ng g⁻¹, and 28 days: 0.39 ng g⁻¹) on account of MeIQx thermolability.     

杭白菊浸膏中香气活性成分分析

香气是评价浸膏质量的重要标准之一,该文为构建浸膏质量标准提供基础数据。采用固相微萃取法(SPME)和溶剂辅助风味蒸发(SAFE)两种前处理方法,结合气相色谱-质谱联用(GC-MS)对杭白菊浸膏的挥发性成分进行了分析,同时采用气相色谱-嗅觉检测技术(GC-O)和香气提取物稀释分析(AEDA)对浸膏中的香味活性成分进行了测定。结果表明:两种前处理方法(SPME和SAFE)结合气质联用仪共检测出119种化合物,醇类30种,酸类6种,酯类28种,醛类4种,酮类12种,烃类36种,其他3种,其中,萜烯类及其含氧衍生物为主要化合物,同时SAFE较SPME法检测到的化合物数量更多;GC-O结合AEDA分析共筛选出35种香气活性成分,风味稀释因子(FD因子)较高的活性成分有芳樟醇(2187)、α-石竹烯(729)、苯乙酸乙酯(729)、己酸乙酯(729)、异戊酸乙酯(729)、α-蒎烯(243)、α-松油醇(243)、异戊酸(243)。     

Volatile fraction of DOP “Castelo Branco” cheese: Influence of breed

“Castelo Branco” cheese is a Portuguese DOP cheese made from raw ewe’s milk coagulated with Cynara cardunculus, ripened for at least 40 days. “Merino da Beira Baixa” pure race is frequently used to produce milk for this cheese, however, exotic races such as Assaf and crusade of these two races are also used. The aim of this work has been to compare the volatile profile and sensory characteristics of DOP “Castelo Branco” cheeses manufactured during winter season with milk of breeds from Merino, Assaf and crusade of these two races and identify volatile compounds that can distinguish these cheeses.     

Volatile compounds on the surface and within Iberian dry-cured loin

The profile of volatile compounds from external and internal areas of Iberian dry-cured loin was studied by headspace solid-phase microextraction. Higher levels of 16 volatile compounds (hexane, decane, 3-methylbutanal, several sulphur compounds and some aromatic hydrocarbons) were detected in the outer part of the loins. These differences could be owing to several factors, such as greater exposure to oxygen and dehydration conditions in the surface of the product, which favour oxidation reactions and Strecker degradation of amino acids. Moreover, the addition of spices on the surface and the proximity of a mould layer growing on the surface of the product could also contribute to the higher levels of these compounds on the external layer. However, other sulphur compounds coming from spices showed similar levels on the surface and within the loins. This different behaviour could be a consequence of different diffusion rates depending on the features of the compound and the matrix.