Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid–liquid microextraction combined with HPLC

A novel, simple, and rapid method is presented for the analysis of aflatoxin B₁, aflatoxin B₂, and ochratoxin A in rice samples by dispersive liquid–liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid–liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B₁ and B₂. Parameters affecting both extraction and dispersive liquid–liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06–0.5 μg/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9–112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China.     

基于手机光线传感器为检测器的简易光度计的自组装设计

By using light sensors of the cellphone, we build a simple photometer which can be used in quantitative analysis experiments. We have performed 5 replicate measurements of iron with phenanthroline to verify reproducibility and stability. We find the absorbance of the sample has a good linear relationship with the concentrations of iron with a R² value around 0.999 and the RSD of 2.81%. The result is 4.94 μg·mL^-1 with spectrophotometer and 5.11 μg·mL^-1 with our photometer. The photometer is simple, convenient, accurate and realistic by using a phone as detector, which can replace the traditional spectrophotometer in the laboratory class. The students can enhance their understanding of the structure and principle of spectrophotometer by the DIY photometer experiment.     

基于FeWOx/SiO2载氧体的甲烷化学链部分氧化反应

甲烷具有价格低廉且储量丰富的优点,因此将甲烷转化为合成气(一种H2:CO为2的混合物),从而进一步合成有价值的化学品和液体燃料引起了人们的极大关注.化学链甲烷部分氧化(CLPOM)技术能避免甲烷与空气直接接触而引起爆炸的危险,可以降低后续对合成气与氮气分离操作所带来的费用,因此日益受到关注.CLOPM过程主要分为两步:第一步,CH4被载氧体所携带的氧部分氧化,载氧体被还原;第二步,利用氧化剂(例如空气)将被还原的载氧体再氧化恢复.因此,载氧体在CLOPM过程中起到至关重要的作用.载氧体的选择主要存在两个问题:(1)甲烷被活化所产生含碳产物的能力与晶格氧的给氧能力不匹配所带来的严重碳沉积;(2)金属离子间扩散速率不匹配而造成载氧体在氧化还原过程中结构的不可逆变化.基于上述两个问题,本文设计了FeWOx/SiO2载氧体用于CLPOM.与未改性的WO3/SiO2载氧体相比,甲烷的转化率和合成气的收率都有显著提高.FeWOx/SiO2在900℃、1 atm反应条件下表现出62%的甲烷转化率、93%的CO气相选择性、94%的H2选择性和2.4的H2/CO比值,同时在50个循环中表现出优异的催化活性和稳定性.本工作利用CH4脉冲反应研究了FeWOx/SiO2的甲烷表面反应过程;采用CH4-TPR和H2-TPR相结合探究了甲烷活化速率与晶格氧扩散速率之间的关系;通过XPS和XRD对FeWOx/SiO2在氧化还原过程中的结构稳定性进行了探讨.综合上述实验结果,对FeWOx/SiO2应用于CLPOM的反应机理进行了阐述.H2-TPR结果表明,在FeWOx/SiO2中,相较于Fe2O3/SiO2,Fe-O的活性受到抑制,使其更倾向于与甲烷发生部分氧化反应;相较于WO3/SiO2,W-O的活性得到明显提升,因此更多的晶格氧可以参与到部分氧化反应中来氧化积碳,从而使合成气收率大幅度提升.从CH4-TPR结果可以看出,对于FeWOx/SiO2,CO与H2的生成温度最接近,意味着晶格氧的传输速率较快并且能够与甲烷活化产生含碳中间物种的速率相匹配,将其及时氧化生成CO,避免由于积碳造成的催化剂失活.结合XPS和XRD结果可以得出,在甲烷还原过程中,FeWOx经历一步还原形成Fe-W合金,由于其间存在强相互作用,因而抑制了还原过程中催化剂相分离现象的发生.同时,根据铁钨离子在空气条件下扩散速率的公式计算可以得出,其相近的离子氧化速率也保证了在氧化过程中催化剂结构的稳定性.本工作为进一步构建用于甲烷化学链部分氧化制合成气的复合金属氧化物载氧体提供了研究思路.     

Recent advances of ambient ionization mass spectrometry imaging in clinical research

The structural information and spatial distribution of molecules in biological tissues are closely related to the potential molecular mechanisms of disease origin, transfer, and classification. Ambient ionization mass spectrometry imaging is an effective tool that provides molecular images while describing in situ information of biomolecules in complex samples, in which ionization occurs at atmospheric pressure with the samples being analyzed in the native state. Ambient ionization mass spectrometry imaging can directly analyze tissue samples at a fairly high resolution to obtain molecules in situ information on the tissue surface to identify pathological features associated with a disease, resulting in the wide applications in pharmacy, food science, botanical research, and especially clinical research. Herein, novel ambient ionization techniques, such as techniques based on spray and solid‐liquid extraction, techniques based on plasma desorption, techniques based on laser desorption ablation, and techniques based on acoustic desorption were introduced, and the data processing of ambient ionization mass spectrometry imaging was briefly reviewed. Besides, we also highlight recent applications of this imaging technology in clinical researches and discuss the challenges in this imaging technology and the perspectives on the future of the clinical research.     

Seeking magneto-structural correlations in easily tailored pentagonal bipyramid Dy(III) single-ion magnets

Science China Chemistry - Controlling molecular magnetic anisotropy via structural engineering is delicate and fascinating, especially for single-molecule magnets (SMMs). Herein a family of...     

MILM hybrid identification method of fractional order neural-fuzzy Hammerstein model

Aiming at the difficult identification of fractional order Hammerstein nonlinear systems, including many identification parameters and coupling variables, unmeasurable intermediate variables, difficulty in estimating the fractional order, and low accuracy of identification algorithms, a multiple innovation Levenberg–Marquardt algorithm (MILM) hybrid identification method based on the fractional order neuro-fuzzy Hammerstein model is proposed. First, a fractional order discrete neuro-fuzzy Hammerstein system model is constructed; secondly, the neuro-fuzzy network structure and network parameters are determined based on fuzzy clustering, and the self-learning clustering algorithm is used to determine the antecedent parameters of the neuro-fuzzy network model; then the multiple innovation principle is combined with the Levenberg–Marquardt algorithm, and the MILM hybrid algorithm is used to estimate the linear module parameters and fractional order. Finally, the academic example of the fractional order Hammerstein nonlinear system and the example of a flexible manipulator are identified to prove the effectiveness of the proposed algorithm.

     

Polyimide separators for rechargeable batteries

Separators are indispensable components of modern electrochemical energy storage devices such as lithium-ion batteries (LIBs).They perform the critical function...     

化学反应-顶空气相色谱法测定气相二氧化硅表面硅羟基

建立了一种基于化学反应-顶空气相色谱测定气相二氧化硅表面硅羟基含量的新方法.实验取气相二氧化硅放入顶空瓶中于105℃烘箱中加热2 h去除水分,将甲苯稀释的格氏试剂注入密闭的顶空瓶中,格氏试剂与气相二氧化硅表面硅羟基快速反应产生甲烷(CH4),甲烷量与气相二氧化硅表面硅羟基含量成正比.经过气相色谱-氢火焰离子化检测器测定...     

延性材料平面冲击波基本实验数值模拟的若干问题

假设屈服强度正比于剪切模量,分别构建了四种强度模型,并用于数值模拟Ly12铝的平面冲击波试验的质点速度剖面以及钨合金的平面冲击波试验的锰铜计应力记录.研究发现,基于Steinberg等的屈服强度模型比较符合实验.还对平面冲击波试验的层裂现象进行了简化的数值模拟,其中,采用了该文作者所提出的一种基于空穴聚集的层裂模型,该模型的特点是分别引入了层裂过程的早期及后期应力松弛方程.     

La1/3Sr2/3Fe1-xCoxO3体系中的Co替代效应研究

本文通过对La1/3Sr2/3Fe1-xCoxO3系列样品进行X射线衍射(XRD)和变温电阻率(p～T)、比热(C～T)、磁化率(M～T)等测试,研究了Co掺杂对该系列样品的晶体结构和电热磁性质的影响.结果表明,随着Co掺杂量的增加,晶胞体积单调减小;电阻中电荷有序(charge ordering,CO)的特征逐渐消失.Co含量低的样品随着温度降低发生顺磁-反铁磁(PM-AFM)转变和金属-绝缘体(M-I)转变;Co含量高的样品则在磁转变温度以下表现出团簇玻璃型短程铁磁有序行为,并且在整个测量温区内具有金属导电特性.这些证明Co掺杂引起电子的局域化效应是导致体系电磁和输运行为发生变化的主要原因.