增敏剂改进超级微波消解-电感耦合等离子体质谱(ICP-MS)法测定食品中硒元素

合适比例增敏剂会对超级微波消解-电感耦合等离子体质谱法(ICP-MS)测定食品中硒元素含量具有一定的优化效果。本文采用超级微波消解仪对1.0 g食品样品进行全消解,采用碰撞池模式规避质谱干扰,内标校正非质谱干扰,选择甲醇、乙醇、乙酸、异丙醇、丙三醇作为增敏剂,并调整测试过程中的添加比例,用电感耦合等离子体质谱法测定。结果表明：2%异丙醇存在时硒元素各同位素响应值最高,其中78Se具有低至0.0003 mg·kg-1的方法检出限;用以上方法对食品标准物质（GSB-8、GSB-9、GSB-24、GSB-30）及实际样品进行分析,标准物质测定值均在其认定值及不确定度范围内,相对误差小于-5.4%;实际样品测定值的相对标准偏差（n=7,RSD）为0.3~1.7%,加标回收率为99.2~105%。本方法操作简便,精密度好,准确度高,可以作为各类食品样品中硒含量测试方法。     

Study of the matrix effects of tetrodotoxin and its content in cooked seafood by liquid chromatography with triple quadrupole mass spectrometry

Tetrodotoxin is a marine biotoxin with high acute toxicity. The levels in cooked seafood will help us to assess its intake in humans and may help assess the risk of toxicity. However, heavy matrices hinder the direct quantitation of tetrodotoxin. A quantitative method of measuring tetrodotoxin in cooked seafood using liquid chromatography with triple quadrupole mass spectrometry was established in this study. Tetrodotoxin was extracted from the sample matrix using 2% formic acid in methanol and cleaned using a cation exchange cartridge. The cleanup conditions were optimized. The matrix effects were determined using the postextraction spiking method and by comparing the slope of the linear regression equation in sample matrix to that in solvent. The limit of detection in the sample matrix was 5 μg/kg and the limit of quantification was 10 μg/kg. The mean recoveries at three spiking levels were 66.9–89.2% with relative standard deviations of 5.0–10.8% (n = 6) in five different matrices. Tetrodotoxin was found at concentrations of 26.1–2462 μg/kg in nine of 83 cooked seafoods tested in this study. Eight analogs of Tetrodotoxin were detected in the samples studied.     

离子色谱的抑制系统及相关技术的发展

抑制系统是抑制型(双柱型)离子色谱系统极为重要的一个组成部分,也是离子色谱有别于其它类型的液相色谱的最重要特点之一。抑制器的发展经历了多个发展时期,而目前商品化的离子色谱仪亦分别采用不同形式的抑制手段。近年来,还发展了一些特殊的辅助抑制器,如接在抑制器后面CO2除去装置,用于提高被测离子的信号或进一步降低背景电导值。     

高温离子热合成MAPO分子筛

在280℃条件下,以磷酸为磷源、异丙醇铝为铝源、乙酸镁为镁源、正二丙胺为结构导向剂,在溴化1-丁基-3-甲基咪唑鎓([BMIM]Br)离子液体中合成了系列MAPO分子筛。随着晶化时间的延长,出现了一个从MAPO-5到MAPO-11、进而到MAPO-25分子筛的转晶过程。这一符合Ostwald定律的转晶过程伴随着骨架密度的增加以及样品形貌和模板剂状态的变化。     

LY12铝疲劳裂纹在冲击载荷下的演化研究

对LY12铝合金在低周疲劳条件下的裂纹情况和随后进行的动态拉伸条件下裂纹的发展给予了观察和统计分析，发现裂纹的累积数密度分布在损伤演化过程中保持指数形式，用NAG模型对实验结果进行分析，得出该材料裂纹演化发展方程的各种参数。     

无机类富勒烯过渡金属硫化物纳米材料的合成及其摩擦学应用研究进展

评述了无机类富勒烯（IF）与过渡金属硫化物（WS2和MoS2等）纳米材料的合成技术及其摩擦学应用研究的最新进展，外型为球形或近似于球形并具有嵌套中空结构的IF－WS2和IF－MoS2纳米果粒具有潜在的摩擦学应用前景；对含有IF－WS2纳米颗粒的复合材料和Ni-P复合镀层的研究表明，其比含有石墨和层状2H－WS2粉末的固体润滑剂具有更优异的摩擦学性能。     

粘塑性薄壁管中复合应力波的传播特性研究

以本构关系一般理论为基础,导出了计及材料功硬化效应和应变率硬化效应的粘塑性薄壁管的本构关系及管中复合应力波的控制方程,应用有限差分方法研究了在压扭复合冲击载荷作用下粘塑性薄壁管中复合应力波的传播特性与演化规律,分析了复合应力波的耦合效应以及薄壁管中粘塑性参数和功硬化效应对复合应力波传播与演化规律的影响,并对有关现象进行了分析和解释。     

Study on detection of mutation DNA fragment in gastric cancer by restriction endonuclease fingerprinting with capillary electrophoresis

The DNA fragment detection focusing technique has further enhanced the sensitivity and information of DNA targets. The DNA fragment detection method was established by capillary electrophoresis with laser‐induced fluorescence detection and restriction endonuclease chromatographic fingerprinting (CE‐LIF‐REF) in our experiment. The silica capillary column was coated with short linear polyarclarylamide (SLPA) using nongel sieving technology. The excision product of various restricted enzymes of DNA fragments was obtained by REF with the molecular biology software Primer Premier 5. The PBR322/BsuRI DNA marker was used to establish the optimization method. The markers were focused electrophoretically and detected by CE‐LIF. The results demonstrate that the CE‐LIF‐REF with SLPA can improve separation, sensitivity and speed of analysis. This technique may be applied to analysis of the excision product of various restricted enzymes of prokaryotic plasmid (pIRES2), eukaryote plasmid (pcDNA3.1) and the PCR product of codon 248 region of gastric cancer tissue. The results suggest that this method could very sensitively separate the excision products of various restricted enzymes at a much better resolution than the traditional agarose electrophoresis. Copyright © 2011 John Wiley & Sons, Ltd.     

Solvent‐Free Aerobic Chemoselective Oxidation of β‐Ionone catalyzed by N‐Hydroxyphthalimide/Co(acac)2

β‐Ionone was oxidized with O₂ under solvent‐free conditions catalyzed by an N‐hydroxyphthalimide/Co(acac)₂ system in mild conditions with high conversion and excellent selectivity to oxo‐β‐ionone or 5,6‐epoxy‐β‐ionone in different reaction conditions, respectively.     

有限元分析中硬化弹塑性本构方程积分算法

基于增量段上的应变关于塑性拉氏乘子的变化率为常矢量的假定,导出一种精确有效的、对有限元分析中线性混合硬化弹塑性本构方程的积分算法。以精确算例和等误差分布图的形式检验了本文方法以及其他两种常用方法的精度。