Method validation for direct determination of some trace and toxic elements in soft drinks by inductively coupled plasma mass spectrometry

The consumption of soft drink beverages has increased in the last few years around the world and it is related to the diversity of brands and flavours available, increasing also the risk of ingestion of compounds considered non-beneficial to the health of consumers. In this study, fast, easy and simple method of analysis for direct determination of As, Pb, Cd, Sb, Hg, Cu, Zn, Fe, Al, Cr, Sn, Co, Mn and Ni in soft drink samples using quadrupole inductively coupled plasma mass spectrometry (Q-ICP–MS) was validated. The estimated detection limits, practical quantification limits, linearity (linear dynamic ranges and method linearity), accuracy (trueness and precision) and measurement uncertainty parameters were studied under optimised (Q-ICP–MS) conditions. The method showed that the estimated detection limits were varied between 0.02 and 2.403 µg/L, and the quantification limits were varied between 0.5 and 20 µg/L. The mean recoveries ± standard deviations at different spiking levels were varied between 75.03 ± 0.62% and 117.07 ± 2.83% and the coefficients of variation were varied between 0.49% and 9.79%. The method trueness was confirmed by using four different certified reference materials (soft drinks and treated water) purchased from FAPAS (Food Analysis Performance Assessment Scheme) and all obtained results were within satisfactory ranges and had acceptable recovery and Z-score values. The method precision, in terms of relative standard deviation, was below 4.88%. The method uncertainty expressed as expanded uncertainty of all validated elements was found to be ≤22.52%. The results obtained make the method suitable for accurate determination of validated elements in different kinds of soft drink samples at these low concentration values. Validated method was used for the determination of metallic contaminants in 40 commercial soft drink samples and the results were compared with the provisional guideline of the elements stated by Egyptian, WHO and European standards in drinking and potable bottled natural mineral water.     

Micro‐ and Nano‐Liquid Phases Coexistent with Ice as Separation and Reaction Media.

Ice has a variety of scientifically interesting features, some of which have not been reasonably interpreted despite substantial efforts by researchers. Most chemical studies of ice have focused on the elucidation of its physicochemical nature and its roles in the natural environment. Ice often contains impurities, such as salts, and in such cases, a liquid phase coexists with solid ice over a wide temperature range. This impure ice also acts as a cryoreactor, governing the circulation of chemical species of environmental importance. Reactions and phenomena occurring in this liquid phase show features different from those seen in normal bulk aqueous solutions. In the present account, we discuss the chemical characteristics of the liquid phase that develops in a frozen aqueous phase and show how novel analytical systems can be designed based on he features of the liquid phase which are predictable in some cases but unpredictable in others.     

高分子材料注塑固化阶段的残余应力分析

在结晶性高分子材料注塑过程的固化阶段，温度分布、材料细观结构和应力应变之间相互耦合，因而其变化规律非常复杂．本文在井上等人考虑材料细观结构变化的金属热加工工艺应力分析［３～６］的基础上，发展了一套用于高分子注塑固化阶段残余应力分析的本构描述和有限元分析方法．在本构模型中，同时考虑了温度变化、结晶和“冻结取向”对变形的贡献．     

ANALYSIS OF MECHANICAL CHARACTERISTICS OF FROZEN CLAY AND MODIFIED S-M CREEP MODEL1)

为合理描述人工冻结法施工的矿井土层力学特性，对某矿井土样的重塑土进行单轴抗压强度实验和单轴压缩蠕变实验，得到重塑冻结黏土在不同温度及载荷加载等级下的应力-应变曲线和蠕变曲线。实验结果表明：冻结温度越低，土样的单轴强度越大；相同冻结温度下，土样的蠕变变形随着应力水平的升高而增大。单轴压缩蠕变的等时应力-应变曲线随时间发展向应变轴靠拢；土样经历初始蠕变和等速蠕变两个阶段，在较高应力水平下有进入加速蠕变的趋势；对S-M模型中各参数的意义进行修正并考虑温度的影响，得到人工冻结黏土改进S-M蠕变显式模型，然后采用粒子群算法对人工冻结黏土S-M蠕变模型参数进行优化。改进S-M蠕变显式模型理论计算值与实验值吻合良好，表明改进S-M蠕变显式模型能较好模拟人工冻结黏土的蠕变特性。改进S-M蠕变显式模型为人工冻土蠕变计算提供一种新方法。     

表面增强拉曼光谱法分析软饮料中的阿斯巴甜

应用超声技术辅助预处理,以纳米银为活性基底,在溶液pH 5.0、纳米银与阿斯巴甜(APM)混合比例1∶1、混合温度30℃、加热时间6 min的条件下,利用表面增强拉曼光谱(SERS)结合化学计量法对纯品及软饮料中APM进行定量检测。结果表明:APM在0.5～100 mg/L范围内线性关系较好,其中水标准溶液的相关系数为0.993 3,检出限(LOD)为0.41 mg/L,苏打水、雪碧、可乐、芬达等标准溶液的相关系数为0.974 7～0.984 8,加标平均回收率为88.4%～121%,相对标准偏差小于7%。运用SERS检测软饮料中APM具有分析速度快、无损、环境污染小等优点,适用于食品中阿斯巴甜的定量分析,为食品添加剂的进一步表征和检测建立了依据,显示了SERS技术在化学物质检测领域具有巨大潜力。     

基于级连相关神经网络的人工冻土本构模型1）

为解决BP (back propagation)神经网络收敛速度慢，网络结构需事先定义等缺点，采用了级连相关神经网络模型来建立人工冻土应力和应变之间的关系。基于该模型推导了冻土的一致刚度矩阵形式，利用人工冻土三轴试验数据对神经网络模型进行训练，并用其替换有限元计算中的传统本构模型，将计算结果与性质及含水率相同的冻土的试验结果进行了对比，发现该神经网络本构模型很好地反应了材料的非线性，能够改善数值计算结果，与实测结果吻合地很好，比具有相同隐含层神经元个数的BP模型更接近实测结果。     

Ultra-High Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry for the Determination of Caffeine in Energy Drinks

A simple and highly sensitive method for the determination of caffeine in energy beverages was developed and validated. Sample preparation utilizing solid-phase extraction (SPE) was simple and reliable. Separation by isocratic ultra-high performance liquid chromatography (UPLC) with a reversed-phase C₁₈ column was performed within 6 min. The use of SPE with UPLC coupled with electrospray ionization-multiple tandem mass spectrometry detection (ESI-MSⁿ) was accurate, reproducible, and validated for the determination of caffeine in energy drink matrices. The limit of quantification for caffeine was approximately 2.1 ng mL^?1. The intra-day and inter-day precisions were less than 4%, and the accuracy of the measurements was between 85.1% and 93.2%. Results for caffeine concentrations in eighteen beverages were compared to the values on the labels. This paper describes the first use of the UPLC–ESI-ion trap MSⁿ technique for quality-control purposes of caffeine present in energy drinks.     

Stabilized finite element method for flows with multiple reference frames

We present a space‐time finite element method capable of dealing with flows in multiple co‐rotating reference frames. Since equal order interpolation is used for all degrees of freedom, Galerkin/least‐squares stabilization is applied. We give a detailed derivation of the equations involved, introduce the variational form, present the stabilization parameters, and also discuss implementation issues. Numerical examples in 2D and 3D show generality and efficiency of the method, if steady‐state behavior of rotating components is sufficient for the CFD analysis. Copyright © 2015 John Wiley & Sons, Ltd.     

阴离子交换树脂结合近红外漫反射光谱测定碳酸饮料中日落黄

采用强碱性阴离子交换树脂富集饮料中的合成食用色素日落黄,用近红外漫反射光谱技术直接测定富集有色素的树脂.将34个模拟样品建模,日落黄浓度范围为0.05～1.2g/L.以柠檬黄和亮丽春红5R为干扰,经偏最小二乘回归建模,得到决定系数为0.9883,标准偏差为0.0187的稳健模型.定量预测3种不同市售饮料中的日落黄,回收...     

人工冻土力学性能影响因素敏感性分析

为分析人工冻土单轴抗压强度影响因素敏感性,选定人工冻土单轴抗压强度的7 种影响因素,按正交试验设计方案进行大量冻土单轴压缩试验,并采用灰色关联理论对试验结果进行分析,研究分析诸因素敏感性排列顺序. 试验结果表明：在选定的7 种影响因素中,温度为最大敏感因素,其它依次为深度、土性、养护时间、加载速率、含水率和密度,且选定的7 种因素均为重要影响因素,为相关室内试验与工程应用提供依据.