Preconcentration sensitive determination of pyrethroid insecticides in environmental water samples with solid phase extraction with SiO2 microspheres cartridge prior to high performance liquid chromatography

Present study developed a new method for the sensitive determination of pyrethroid insecticides with solid phase extraction in combination with high performance liquid chromatography and UV detector. SiO₂ microspheres, a new SiO₂ based material, was investigated for the enrichment ability and applicability as the solid phase extraction sorbent. Four pyrethroid pesticides such as fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were used as the target analytes. Parameters that maybe influence the extraction efficiency such as the eluent type and its volume, sample flow rate, sample pH, and the sample volume were optimized in detail, and the optimal conditions were as followed: sample volume, 100 mL; concentration of methanol, 30%; acetone volume, 5 mL; sample flow rate, 4.2 mL min⁻¹; sample pH, 7. The experimental results indicated that there was good linearity in the concentration range of 0.1–50 μg L⁻¹ except biphenthrin in the range of 0.05–25 μg L⁻¹. The detection limits for fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were in the range of 0.02–0.08 μg L⁻¹. The intra-day and day to day precisions (RSDs, n = 6) were in the ranges of 2.6–4.4% and 5.3–7.2%, respectively. The method was validated with five real environmental water samples, and all these results proved that proposed method could be used as a good alternative for the routine analysis for such pollutants in environmental samples.     

低阻抗脉冲形成网络引线电感的模拟及实验研究

 对2.5 Ω,200 ns低阻抗Blumlein型脉冲形成网络进行3维建模,利用有限元仿真软件,分别采用静电场分析方法及高频分析方法对开关端、负载端的电感进行模拟研究,结果表明:随着工作频率增大,引线电感值逐渐减小,工作频率为2.5 MHz时,引线内电感可以忽略不计。此时模拟得到的引线电感要比静态模拟结果小10 nH左右;两个开关并联工作时不仅要考虑引线自身的电感,还要考虑同步导通时互感的影响,且互感达到了自感的1/4。使用Pspice软件对模拟结果进行仿真,采用电磁屏蔽后输出波形前沿相对于屏蔽前输出波形前沿要小2.1 ns。实验研究结果表明,采用电磁屏蔽前后输出波形的前沿分别为68.8,65.2 ns,减小量与模拟结果基本吻合。     

用特征多项式构造相移干涉相位提取算式

用相移干涉术测量物体表面形貌时，各种误差因素特别是相移器移相误差的影响使得表面形貌的测量偏离了实际值，甚至会产生形貌失真的现象。采用傅里叶分析的方法对相位提取算式作了理论分析，并根据特征多项式设计分析理论构造了新的、对移相误差不敏感的相位提取算式。经实验验证，该算法有效地提高了相移干涉仪测量表面形貌的Ra值，重复测量精度达5倍以上，使测量结果更接近实际值。     

一种高性能小周期摇摆器

介绍一种高性能小周期摇摆器的设计。采用槽型定位的分离状磁块,实现了磁场的半周期调节,对该摇摆器模型进行的测量表明,当摇摆器的周期λ_w=10mm,磁极间隙δ为5mm时,峰值磁场B_w=0.35T,磁场最大偏差δB_w/B_w<1.25％。     

3，5－二溴－4－氨基苯基荧光酮的离解及与钼显色反应的研究

用分光光度法研究了２，３，７－三羟基－９－（３，５－二溴－４－氨基）苯基荧光酮的离解平衡和离解常数；以其为显色剂，进行了钼（ＶＩ）的分光光度法研究，在０．２～０．８ｍｏｌ·Ｌ－１ＨＣｌ溶液中，ＣＴＭＡＢ存在下，显色剂与Ｍｏ（ＶＩ）生成灵敏的红色三元配合物，ε５３０＝１．５６×１０５Ｌ·ｍｏｌ－１·ｃｍ－１，用于测定钢中的钼，结果满意．     

Radiobiological response of human hepatoma and normal liver cells exposed to carbon ions generated by Heavy Ion Research Facility in Lanzhou

Human hepatoma and normal liver cells were irradiated with ¹²C⁶⁺ ion beams (LET = 96.05 keV/μm) and γ-rays at Heavy Ion Research Facility in Lanzhou (HIRFL). The chromatid breaks and break types were detected using the premature chromosome condensation technique. Our experimental results showed that chromatid breaks seem to have a good relation with ¹²C⁶⁺ absorbed dose and ¹²C⁶⁺ are more effective to induce chromatid breaks as compared to the γ-rays. For ¹²C⁶⁺ ion irradiation the major break was isochromatid break, while chromatid breaks were dominant for γ-ray irradiation. We also observed that the Relative Biology Effectiveness (RBE) of ¹²C⁶⁺ ion is about 2.5 times higher than that of γ-rays.     

Phenylmethanesulfonyl fluoride pretreatment stabilizes plasma lipidome in lipidomic and metabolomic analysis

Though it is standard practice to test the stability of analytes in the matrix for routine bioanalytical method, stability evaluation is always impractical and skipped in untargeted lipidomic and metabolomic analysis because analytes in these studies are enormous, diverse and sometimes unknown. Lipidome represents a major class of plasma metabolome and shows great potential to be diagnostic and prognostic biomarkers. However, lipidome also faces stability problems because plasma contains kinds of lipid degradation enzyme. Here, using liquid chromatography time of flight mass spectrometry based lipidomic methodology, plasma levels of various lipids including triglyceride (TG), diglyceride (DG), free fatty acid (FFA), phosphatidylethanolamine (PE) phosphatidylcholine (PC), lyso-phosphatidylcholine (LPC), lyso-phosphatidylethanolamine (LPE), and sphingomyelin (SM) were dynamically determined within 4 h at ambient temperature. In mouse and rat plasma, the levels of most TG, DG, PC and PE species significantly decreased with respect to time, whereas those of LPC, LPE and FFA significantly increased with respect to time. However, such changes did not occur in human plasma, thus indicating hepatic lipase and esterase might involve in the species-specified degradation of lipid classes in plasma. Phenylmethanesulfonyl fluoride (PMSF) pretreatment prevented such lipidome instability in mouse plasma. The results suggested the instability of plasma lipidome should be highly concerned, and the enhancement of ex vivo stability of plasma lipidome could enable more reliable clinical translation of lipidomic data for biomarker discovery.     

Determination of phthalate esters from environmental water samples by micro‐solid‐phase extraction using TiO2 nanotube arrays before high‐performance liquid chromatography

We describe a highly sensitive micro‐solid‐phase extraction method for the pre‐concentration of six phthalate esters utilizing a TiO₂ nanotube array coupled to high‐performance liquid chromatography with a variable‐wavelength ultraviolet visible detector. The selected phthalate esters included dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, bis(2‐ethylhexyl)phthalate and dioctyl phthalate. The factors that would affect the enrichment, such as desorption solvent, sample pH, salting‐out effect, extraction time and desorption time, were optimized. Under the optimum conditions, the linear range of the proposed method was 0.3–200 μg/L. The limits of detection were 0.04–0.2 μg/L (S/N = 3). The proposed method was successfully applied to the determination of six phthalate esters in water samples and satisfied spiked recoveries were achieved. These results indicated that the proposed method was appropriate for the determination of trace phthalate esters in environmental water samples.     

Double-stranded ladderphanes with C2-symmetric planar chiral ferrocene linkers

Eight ladderphanes with C₂-symmetric planar chiral ferrocene linkers are synthesized by ring opening metathesis polymerization of bisnorbornene monomers using Grubbs-I catalyst. The aminobenzoate in both monomers and polymers shows absorption maximum around 320 nm. Both monomers and polymers are Circular dichroism (CD) active. Little enhancements of CD profiles around 320 nm are observed for ladderphanes having chiral chloro- or phenyl-substituted ferrocene linkers. However, ladderphanes with a phenyl substituent on the cyclopendienyl ring exhibits enhancement of CD curves aound 240–300 nm. The congested phenyl moieties in adjacent linkers in this polymer might be well oriented such that interactions between these aromatic substituents on different monomeric units might provoke the enhancement of the CD curves in this region. When the methyl-substituted cyclopendienyl ligand is used for chiral ferrocene linkers, the ladderphanes exhibit two-fold enhancement of CD spectrum around 320 nm. This enhancement is further increased when the cyclopentadienyl ligand contains an additional phenyl substituent, owing to exciton coupling between aminobenzoate moieties in adjacent monomeric units. Moreover, the intensity of the CD curves in the region of 240–300 nm is significantly increased. These results suggest that the later polymer may adopt a posible helical structure. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 2999–3010     

异丁烷直接脱氢制异丁烯催化剂研究进展

从热力学和反应机理角度概述了异丁烷直接脱氢和氧化脱氢的差异;从活性中心性质、失活与再生、助催化剂以及载体方面,综述了目前广泛研究的异丁烷直接脱氢制异丁烯催化剂,包括PtSn-、CrOx-、GaOx基和金属硫化物催化剂,并分析了各类催化剂的优缺点及目前的研究方向;简述了其他类型的脱氢催化剂,包括Mo/MgAl2O4、碳基材料、Co-、Ni2P-、VOx基催化剂等;分析了目前脱氢技术面临的问题以及未来的研究方向。