Simultaneous voltammetric determination of carbendazim and carbaryl in medicinal plant infusions with a boron-doped diamond electrode

This study is aimed to develop an electroanalytical methodology using a boron-doped diamond electrode to determine simultaneously and selectively carbendazim (CBZ) and carbaryl (CAR). In previous studies using cyclic voltammetry oxidation, peaks were observed at 1.03 V (CBZ) and 1.44 V (CAR), with characteristics of an irreversible process controlled by diffusion of species, with a supporting electrolyte of BR buffer (0.1 mol L^?1) and pH adjusted to 6.0. The differences between the potentials for both pesticides, about 400 mV, indicate the possibility of selective determination of CBZ and CAR. The square-wave voltammetric parameters were optimised. The best separation conditions were pH 6.0, square-wave frequency of 100 s^?1, pulse amplitude of 50 mV and scan increment of 2.0 mV. These parameters were used to obtain the calibration curves of CBZ and CAR. An analytical curve was constructed in the range concentration of CBZ of 1.3 mg L^?1 to 15.3 mg L^?1 and CAR of 1.0 mg L^?1 to 11.4 mg L^?1, respectively. The limits of detection (LOD) and limits of quantification (LOQ) for CBZ were 0.40 mg L^?1 and 1.30 mg L^?1, respectively. For CAR, the LOD and LOQ were 0.30 mg L^?1 and 1.00 mg L^?1, respectively. Sensitivity values were 0.78 and 2.60 µA/mg L^?1 for CBZ and CAR, respectively. The electroanalytical method was applied in Mikania glomerata infusions. The recovery values were 106.2% and 116.5% for CBZ and CAR, respectively. The results show that the developed method is suitable for application in medicinal plant samples.     

Banach空间中太阳集对无穷序列的最佳同时逼近

本文研究太阳集对一列无穷序列的最佳同时逼近问题，建立了特征及唯一性结果．     

基于二维光栅分光的同步移相干涉测量技术

为了干涉测量的抗振目的,提出了一种新的同步移相干涉测量方案并搭建了实验装置。整个测量系统在迈克耳孙偏振移相干涉仪的基础上,利用一个正交的二维光栅产生对称分光,选取对于理想光栅衍射效率一致的(±1,±1)级衍射光作为测量分光路,使之分别通过偏振方向依次相差45°的一个偏振片组,从而分别形成0°、90°、180°和270°相移的四幅移相干涉图,按照传统的四步移相算法,对被测波面进行了复原。分析了光强畸变和移相误差对系统的测量误差的影响。利用该系统测量一球面系统,结果与在ZYGO干涉仪上相比较,球面系统的均方根误差相差0.012λ,峰谷值相差0.051λ。     

关于K-分块循环矩阵及其对角化问题的讨论

给出了K-分块循环矩阵的概念,并探讨了K-分块循环矩阵的相似类及其对角化问题.     

液相色谱-串联质谱法同时测定大黄鱼中20种磺胺类药物残留

建立了一种液相色谱-电喷雾串联质谱同时测定大黄鱼中20种磺胺类药物残留的方法.均质样品先后用乙腈、二氯甲烷提取,合并提取液,取部分提取液经氮吹浓缩.残渣用1 mL流动相溶解,饱和正己烷脱脂净化.采用ZORBAX Eclipse XDB-C8色谱柱,以含0.2%乙酸的水溶液和甲醇(7: 3)为流动相,梯度洗脱,在电喷雾-多反应监测离子模式下,进行定量定性分析.方法的定量限为5 μg/kg;以标准加入法计算回收率,在10～40 μg/kg添加范围内,平均回收率为79.6%～109%;相对标准偏差为3.55%～16.5%.     

An eigen-based high-order expansion basis for structured spectral elements

We present an eigen-based high-order expansion basis for the spectral element approach with structured elements. The new basis exhibits a numerical efficiency significantly superior, in terms of the conditioning of coefficient matrices and the number of iterations to convergence for the conjugate gradient solver, to the commonly-used Jacobi polynomial-based expansion basis. This basis results in extremely sparse mass matrices, and it is very amenable to the diagonal preconditioning. Ample numerical experiments demonstrate that with the new basis and a simple diagonal preconditioner the number of conjugate gradient iterations to convergence has essentially no dependence or only a very weak dependence on the element order. The expansion bases are constructed by a tensor product of a set of special one-dimensional (1D) basis functions. The 1D interior modes are constructed such that the interior mass and stiffness matrices are simultaneously diagonal and have identical condition numbers. The 1D vertex modes are constructed to be orthogonal to all the interior modes. The performance of the new basis has been investigated and compared with other expansion bases.     

Single‐run capillary electrophoresis method for the fast simultaneous determination of amoxicillin,clavulanate, and potassium

We report a new fast method for the simultaneous determination of amoxicillin, clavulanate, and potassium by capillary electrophoresis with capacitively coupled contactless conductivity detection. Samples containing potassium as the cation, and both amoxicillin and clavulanate as anions were determined simultaneously in a single run (in less than 45 s) using 10 mmol/L of both 2‐amino‐2‐hydroxymethyl‐propane‐1,3‐diol and 3‐{[2‐hydroxy‐1,1‐bis(hydroxymethyl)ethyl]amino}‐1‐propanesulfonic acid (pH 8.4) as the background electrolyte. Limits of detection were 25.0, 5.0, and 4.0 μmol/L for amoxicillin, clavulanate, and potassium, respectively. The proposed method is inexpensive, simple, fast (75 injections h⁻¹), environment friendly (minimal waste generation), and accurate (recovery values between 98 and 103%). The results obtained with the proposed method were statistically similar (95% confidence level) to those obtained by using high‐performance liquid chromatography (amoxicillin and clavulanate) and flame photometry (potassium).     

Highly selective coextraction of rhodamine B and dibenzyl phthalate based on high‐density dual‐template imprinted shells on silica microparticles

A simple one‐pot approach based on molecularly imprinted polymer shells dispersed on the surface of silica for simultaneous determination of rhodamine B and dibenzyl phthalate (DBzP) has been developed. Highly dense molecularly imprinted polymer shells were formed in the mixture of acetonitrile and toluene by the copolymerization of methacrylic acid and ethylene glycol dimethacrylate, as well as two templates, rhodamine B and dibenzyl phthalate, directed by the vinyl end groups functional monolayer at surface silica microspheres after 3‐methacryloxypropyl trimethoxysilane modification. The obtained imprinted polymer shells showed large average pore diameter (102.5 nm) and about 100 nm shell thickness. The imprinted particles also showed high imprinting factor (α_RhB = 3.52 and α_DBzP = 3.94), rapid binding kinetics, and excellent selective affinity capacity for rhodamine B and dibenzyl phthalate containing another three competitors in mixed solution. Moreover, the imprinted particles coupled with ultra high performance liquid chromatography was successfully applied to simultaneous analysis of rhodamine B and dibenzyl phthalate in two spiked beverage samples with average recoveries in the range of 88.0−93.0% for rhodamine B and 84.0–92.0% for dibenzyl phthalate with the relative standard deviation lower than 5.1%.     

Systematic Study of Selected Diagonalization Methods for Configuration Interaction Matrices

Several modifications to the Davidson algorithm are systematically explored to establish their performance for an assortment of configuration interaction (CI) computations. The combination of a generalized Davidson method, a periodic two‐vector subspace collapse, and a blocked Davidson approach for multiple roots is determined to retain the convergence characteristics of the full subspace method. This approach permits the efficient computation of wave functions for large‐scale CI matrices by eliminating the need to ever store more than three expansion vectors ( b _i) and associated matrix‐vector products ( σ _i), thereby dramatically reducing the I/O requirements relative to the full subspace scheme. The minimal‐storage, single‐vector method of Olsen is found to be a reasonable alternative for obtaining energies of well‐behaved systems to within μE_h accuracy, although it typically requires around 50% more iterations and at times is too inefficient to yield high accuracy (ca. 10^?10 E_h) for very large CI problems. Several approximations to the diagonal elements of the CI Hamiltonian matrix are found to allow simple on‐the‐fly computation of the preconditioning matrix, to maintain the spin symmetry of the determinant‐based wave function, and to preserve the convergence characteristics of the diagonalization procedure. © 2001 John Wiley & Sons, Inc. J Comput Chem 22: 1574–1589, 2001     

Sensitivity-enhanced sim-CT HMQC PFG-HBHA(CO)NH and PFG-CBCA(CO)NH triple-resonance experiments

Short transverse relaxation times of Calpha and Cbeta single-quantum coherences reduce the sensitivity of triple-resonance experiments involving transfers of Calpha/Cbeta or Halpha/Hbeta coherences. Multiple-quantum line-narrowing techniques improve the relaxation properties of 13C coherences, thereby increasing the sensitivity of the experiment. In the present work, we describe PFG-CBCA(CO)NH and PFG-HBHA(CO)NH experiments that utilize heteronuclear multiple-quantum coherences in a simultaneous constant-time period to obtain completely decoupled spectra with improved sensitivity. Results indicate that approximately 30% of cross peaks show an average enhancement of approximately 15% in the CBCA(CO)NH experiment. In the related HBHA(CO)NH experiment, approximately 97% of the cross peaks show an average enhancement of approximately 40%.