Application of thermal ultrasound-assisted liquid–liquid micro-extraction coupled with HPLC-UV for rapid determination of synthetic phenolic antioxidants in edible oils

A simple, fast, and reliable liquid–liquid micro-extraction (LLME) method assisted by thermal ultrasound approach was developed for simultaneous determination of synthetic phenolic antioxidants (SPAs) in edible oils by high-performance liquid chromatography equipped with ultraviolet detector (HPLC-UV). The synthetic antioxidants were propyl gallate (PG), butylated hydroxyanisole (BHA), tert-butylhydroquinone (TBHQ), and butylated hydroxyltoluene (BHT). The best extraction conditions were observed were methanol/acetonitrile (1:1, v/v) as the solvent, ultrasound at 4 min, and a temperature of 40°C. The linearity of the calibration curves for the optimum conditions were R² > 0.989 for all of the SPAs in a range from 1–200 μg ml⁻¹. Relative standard deviation (RSD %) for five analysis was in range of 2.83% to 4.21%. Limit of detection (LOD) and limit of quantification (LOQ) were obtained in range of 0.012–0.06 and 0.04–0.2 μg g⁻¹, respectively. With regard to recovery, a range of 91%–116% was calculated for the spiked edible oils.     

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.     

不同品种金针菇特征挥发性物质的差异分析

采用顶空固相微萃取-气相色谱-质谱(solid phase micro-extraction-gas chromatography-mass spectrometry,SPME-GC-MS)联用技术和电子鼻技术对金针菇5 个品种川金3号、川金11号、川金54号、L4和L7中的挥发性物质进行鉴定并定量分析,并结合主成分分...     

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。     

不同方法提取艾纳香叶挥发性成分的气相色谱-质谱分析

采用气相色谱-质谱法(GC-MS)分析水蒸汽蒸馏法(SD)、同时蒸馏萃取法(SDE)和顶空固相微萃取法(HS-SPME)3种方法提取的艾纳香叶挥发性成分。结果表明:3种方法提取艾纳香叶挥发性成分中主要是醇类和烯类化合物,其中萜类物质占较大比例。3种方法的提取物中分别鉴定出化合物50种(SD)、24种(SDE)和49种(HS-SPME)。水蒸汽蒸馏法和同时蒸馏萃取法提取的油状挥发物中主要成分相似,水蒸汽蒸馏法提取油状挥发物与顶空固相微萃取法提取挥发性成分的种类和相对含量相似,同时蒸馏萃取法提取油状挥发物中低沸点化合物较少。     

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.     

不同超高压处理压力对哈密瓜汁香气的影响

采用固相微萃取方法对不同超高压处理的哈密瓜汁的香气进行富集 ,并经GC MS联机检索分析 ,发现超高压处理对哈密瓜汁中的酯类、醇类、醛类和酮类都有影响 ,其中超高压处理哈密瓜汁的酯类减少了 5种且峰面积减少了约 10 % ,而醛类和酮类增加。 5 0 0MPa/2 0min处理的哈密瓜汁与 40 0MPa/2 0min处理的哈密瓜汁相比 ,酯的种类和峰面积变化不大 ,酮的种类没有变化 ,但增加了 3种不饱和醛。 2种超高压条件处理的哈密瓜汁酯类的特征香气成分未变 ,但醇类和醛类的特征香气成分变化较大。感官评定表明 :超高压处理的哈密瓜汁的香气减弱 ,青鲜气增强 ,这与哈密瓜汁香气成分检测的结果相符合。     

中温杀菌对乳化肠挥发性风味物质变化的影响

以乳化肠为研究对象,分析中温杀菌与低温、高温杀菌带来的风味物质的变化规律。利用固相微萃取-气相色谱-质谱联用仪,分别对80℃低温杀菌、95℃中温杀菌、105℃中温杀菌和121℃高温杀菌的乳化肠的挥发性风味成分进行定性和半定量的分析。结果表明:4种热杀菌的乳化肠分别鉴定出39、39、41、37种挥发性风味物质,不同的热杀菌方式会导致挥发性风味物质种类和含量发生变化;对中温乳化肠风味贡献较大的化合物有:己醛、壬醛、1-辛烯-3-醇、2-戊基呋喃和2-甲氧基-4-(2-丙烯基)-苯酚。