Generic applications of 13C‐detected NMR diffusion to formulated systems with suppression of thermal convection induced by proton decoupling

Fast and effective structural/compositional analysis on formulated systems represents one of the major challenges encountered in analytical science. ¹³C‐detected diffusion represents a promising tool to tackle the aforementioned challenges, particularly in industry. Toward exploring the generic applications of ¹³C‐detected diffusion, thermal convection induced by ¹H decoupling has been identified as a key factor that resulted in significantly reduced resolution in the diffusion dimension. Optimization of experimental parameters and utilization of double‐stimulated echo‐based pulse sequence both can effectively suppress the thermal convection caused by the ¹H decoupling, the success of which allows robust and generic applications of ¹³C‐detected diffusion to systems from mixtures of small molecules, polymer blends, and copolymers to actual complex formulated systems. The method is particularly powerful in differentiating small molecules from polymers, polymer blends from copolymers, and end‐group analysis. Copyright © 2016 John Wiley & Sons, Ltd.     

Transferkoeffizienten im System Boden—Pflanze in verschiedenen Lokalitäten der Tschechoslovakei

Für die Ermittlung der Transferkoeffizienten im System Boden–Pflanze wurden in drei Stellen der Tschechoslovakei Boden- und Pflanzenproben entnommen. Die niedrigsten Transferkoeffizienten für Getreide und für mehrjährige Futterpflanzen wurden in der Ostslovakei festgestellt. Die Werte der Transferkoeffizienten waren durch den Bodentyp, den Gesamt-Sorptionskapazität und dem Grad der Sorptionssättigung beeinfluβt.

Soil and plant samples were sampled for the determination of soil to plant transfer coefficients in three various Czechoslovak sites. The lowesl transfer factors for cereals and fodder were determined in the site of Eastern Slovakia. Values of transfer factors depend on soil type, cation exchange capacity and base saturation of soils.     

UPLC - ESI MS/MS法测定动物饲料中苯二氮卓类药物

建立了超高效液相色谱-电喷雾串联质谱(UPLC - ESI MS/MS)同时检测动物饲料中地西泮、奥沙西泮、硝西泮、三唑仑、艾司唑仑和咪达唑仑6种苯二氮卓类药物的方法.饲料样品采用碱性叔丁基甲醚提取,Oasis MCX固相萃取柱净化,反相色谱柱分离,以0.1％甲酸和乙腈为流动相进行梯度洗脱,正离子模式扫描,多反应监测模...     

参数化滤波器逼近问题的棱柱算法

本文基于多胞形上D.C.函数的棱柱算法,给出了一维参数化小波滤波器逼近问题的一种算法.     

阵列馈源偏置抛物面天线合成高功率微波的研究

 运用物理光学分析方法，对使用7单元的扇形喇叭一维阵列和角锥喇叭或圆锥喇叭三角形阵列喇叭束作为单偏置抛物面天线的馈源，空间合成高功率微波进行了比较研究，数值分析表明在阵元输入功率、口面最大场强、天线口径、净空间及天线边缘照度相同,且阵列馈源具有准轴对称主瓣条件下，扇形喇叭构成的一维阵列馈源与单偏置抛物面组成的天线系统的方向性系数和溢出效率优于采用角锥喇叭三角形阵列馈源或圆锥喇叭三角形阵列馈源的天线系统。若将喇叭束直接作为辐射天线使用，由于圆锥喇叭三角形阵列方向性系数对阵元间相位波动的稳定性较好，而更具优势。     

固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留

建立了采用固相萃取-液相色谱-质谱/质谱(SPE-LC-MS/MS)对蜂蜜中磺胺类、硝基咪唑类、喹诺酮类、大环内酯类、林可酰胺类和吡喹酮共计6大类54种药物残留同时测定的方法。蜂蜜经磷酸盐缓冲溶液(pH 8)稀释,Oasis HLB固相萃取柱净化后,通过液相色谱-质谱联用技术进行检测(正离子方式,多反应监测模式)。采用同位素稀释内标法或外标法进行定量,线性关系良好,相关系数大于0.992。方法的定量限(LOQ,以信噪比(S/N)大于10计)分别为磺胺类和硝基咪唑类药物1.0 μg/kg,喹诺酮类和林可酰胺类药物2.0 μg/kg,大环内酯类药物3.0 μg/kg,吡喹酮0.3 μg/kg。总体回收率为32.6%～114%,相对标准偏差为1.3%～28.9%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为蜂蜜中相关药物残留量的筛选检测方法。     

Rapid determination of organochlorine pesticide residues in feeds by capillary gas chromatography

A simple micro-method is described for determination of 15 organochlorine pesticide residues in mixed feeds. Clean-up of the petroleum ether extract is by basic alumina minicolumn chromatography and quantitative identification is by capillary gas chromatography with electron capture detection. Cyanopropyl-polysiloxane chemically bonded fused silica capillary columns have been used to perform high resolution analyses in short time as well as to overcome possible interferences by PCBs. Recovery, repeatability, and detection limits of the proposed procedure are checked and results are also reported for non random samples of 180 feeds collected in Italy.     

A novel highly flexible,simple, rapid and low-cost fabrication tool for paper-based microfluidic devices (μPADs) using technical drawing pens and in-house formulated aqueous inks

Paper-based microfluidic devices (μPADs) are capable of achieving rapid quantitative measurements of a variety of analytes inexpensively. μPADs rely on patterning hydrophilic-hydrophobic regions on a sheet of paper in order to create capillary channels within impermeable fluidic brakes on the paper. Here, we present a novel, highly flexible and low-cost fabrication method using a desktop digital craft plotter/cutter and technical drawing pens with tip size of 0.5 mm. The pens were used with either commercial black permanent ink for drawing fluidic brakes, or with specialty in-house formulated aqueous inks. With the permanent marker ink it was possible to create barriers on paper rapidly and in a variety of designs in a highly flexible manner. For instance, a design featuring eight reservoirs can be produced within 10 s for each μPAD with a consistent line width of brakes (%RSD < 1.5). Further, we investigated the optimal viscosity range of in-house formulated inks controlled with additions of poly(ethylene glycol). The viscosity was measured by capillary electrophoresis and the optimal viscosity was in the range of ∼3–6 mPa s. A functional test of these μPADs was conducted by the screening of antioxidant activity. Colorimetric measurements of flavonoid, phenolic compounds and DPPH free radical scavenging activity were carried out on μPADs. The results can be detected by the naked eye and simply quantified by using a camera phone and image analysis software. The fabrication method using technical drawing pens provides flexibility in the use of in-house formulated inks, short fabrication time, simplicity and low cost.     

超高效液相色谱-电喷雾串联质谱法测定动物饲料中的大环内酯类和林可胺类抗生素

建立了动物饲料中竹桃霉素、红霉素、吉他霉素、交沙霉素、罗红霉素、泰乐菌素6种大环内酯和林可霉素、克林霉素2种林可胺抗生素的超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)检测方法。饲料样品采用甲醇提取,Oasis HLB固相萃取柱富集净化,Waters Acquity UPLC BEH C18色谱柱分离,以0.1%甲酸和乙腈为流动相进行梯度洗脱,流速为0.3 mL/min,正离子模式扫描,多反应监测模式检测,外标法定量。实验结果表明,8种药物在1～100 μg/L范围内具有良好的线性关系。在空白饲料样品中分别添加1、10和100 μg/kg 3个加标水平的8种药物,其平均回收率为68.6%～95.2%,相对标准偏差(RSD)为4.9%～11.8%,定量限均为1 μg/kg。结果表明,该方法简便快速、灵敏度高,适用于动物饲料中大环内酯类和林可胺类抗生素的同时检测。     

Frequency-invariant robust adaptive beamforming based on interference covariance matrix reconstruction

Consider the problems of frequency-invariant beampattern optimization and robustness in broadband beamforming.Firstly,a global optimization algorithm,which is based on phase compensation of the array manifolds,is used to construct the frequency-invariant beampattern.Compared with some methods presented recently,the proposed algorithm is not only available to get the global optimal solution,but also simple for physical realization.Meanwhile,a robust adaptive broadband beamforming algorithm is also derived by reconstructing the covariance matrix.The essence of the proposed algorithm is to estimate the space-frequency spectrum using Capon estimator firstly,then integrate over a region separated from the desired signal direction to reconstruct the interference-plus-noise covariance matrix,and finally caleulate the adaptive beamformer weights with the reconstructed matrix.The design of beamformer is formulated as a convex optimization problem to be solved.Simulation results show that the performance of the proposed algorithm is almost always close to the optimal value across a wide range of signal to noise ratios.