Inverse colloidal crystal membranes for hydrophobic interaction membrane chromatography

A collaborative study on the robustness and portability of a capillary electrophoresis‐mass spectrometry method for peptide mapping was performed by an international team, consisting of 13 independent laboratories from academia and industry. All participants used the same batch of samples, reagents and coated capillaries to run their assays, whereas they utilized the capillary electrophoresis‐mass spectrometry equipment available in their laboratories. The equipment used varied in model, type and instrument manufacturer. Furthermore, different types of sheath‐flow capillary electrophoresis–mass spectrometry interfaces were used. Migration time, peak height and peak area of ten representative target peptides of trypsin‐digested bovine serum albumin were determined by every laboratory on two consecutive days. The data were critically evaluated to identify outliers and final values for means, repeatability (precision within a laboratory) and reproducibility (precision between laboratories) were established. For relative migration time the repeatability was between 0.05 and 0.18% RSD and the reproducibility between 0.14 and 1.3% RSD. For relative peak area repeatability and reproducibility values obtained were 3–12 and 9–29% RSD, respectively. These results demonstrate that capillary electrophoresis‐mass spectrometry is robust enough to allow a method transfer across multiple laboratories and should promote a more widespread use of peptide mapping and other capillary electrophoresis‐mass spectrometry applications in biopharmaceutical analysis and related fields.     

The Crystal Structure and Synthesis Mechanism of 3,6‐Bis(3,5‐dimethylpyrazol‐1‐yl)‐1,4‐dihydro‐1,2,4,5‐tetrazine (BDT): A Key Precursor of S‐tetrazine

The single crystal structure of 1,1′‐bis (3,5‐dimethyl‐pyrazole) methenehydrazine (BDM) was determined by X‐ray single crystal diffraction for the first time. The obtained experimental results indicated that BDM was the intermediate of 3,6‐bis(3,5‐dimethylpyrazol‐1‐yl)‐1,4‐dihydro‐1,2,4,5‐tetrazine (BDT), which was the key precursor of s‐tetrazine. By this evidence, the preparation mechanism of BDT was proved: At 318.15 K, triaminoguanidine and pentanedione reacted to achieve the intermediate (BDM) by molecular nucleophilic addition and intramolecular nucleophilic substitution; when heated to 363.15 K, BDT was then generated by two molecules of BDM with nucleophilic substitution reaction. Furthermore, the thermal decomposition properties and also the non‐isothermal kinetic parameters have been investigated in the present work.     

Simultaneous determination of triazine herbicides in rice by high-performance liquid chromatography coupled with high resolution and high mass accuracy hybrid linear ion trap-orbitrap mass spectrometry

A method was developed for the simultaneous determination of 10 triazine herbicides (cyanazine, simazine, simetryn, metribuzin, atrazine, ametryn, terbuthylazine, prometryn, terbutryn, and dimethametryn) in rice samples by high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer. After extraction with acetonitrile and evaporation, the herbicides were redissolved in n-hexane and purified on a Florisil solid-phase extraction column. All compounds were separated within 12 min, producing more than 11 data points for each herbicide and high mass accuracy quantified ions which the mass errors of absolute value were less than 1.9 ppm in pure solution and 2.1 ppm in the matrix-matched standards solution. The method was validated in terms of the limits of detection and the limits of quantification. The linearity was satisfactory, with a correlation coefficient of >0.9975. Precision and recovery studies were evaluated at three concentration levels for Japonica, Indica, and Glutinous rice matrix. The mean recoveries obtained for all analytes in spiked Xiushui 03, Liangyoupeijiu, and Taihunuo rice samples were 83.3–99.0%, 82.0–99.7%, and 84.2–99.4%, respectively, with relative standard deviation in range 1.7–10.6%, 1.2–10.7%, and 1.9–11.6% for spiked rice samples, respectively. The intra-day precision (n = 5) for the 10 herbicides in rice samples spiked at an intermediate level was between 2.8% and 7.9%, and the inter-day precision over 10 days (n = 10) was between 5.5% and 15.9%.     

A general copper powder-catalyzed Ullmann-type reaction of 3-halo-4(1H)-quinolones with various nitrogen-containing nucleophiles

3-(N-Substituted) 4(1H)-quinolinones were synthesized using the copper-catalyzed Ullmann C-N bond forming strategy in moderate to quantitative yields. Starting from 3-halo-4(1H)-quinolones, various nucleophiles including amides, lactams, sulfonamides and NH-containing azoles have been used successfully. In all cases, the reactions take place rapidly in toluene and proceed by using copper powder as a catalyst, DMEDA as a ligand and K(2)CO(3) as a base. In addition, other related heterocycles such as 3-bromoquinolin-2(1H)-ones, 3-bromocoumarin, and 3,5-dibromo-2-pyridone show good to very high reactivity with various nucleophiles under our Cu/DMEDA catalyst system.     

An optimal replenishment policy for deteriorating items with time-varying demand and partial backlogging

Recently, Papachristos and Skouri developed an inventory model in which unsatisfied demand is partially backlogged at a negative exponential rate with the waiting time. In this article, we complement the shortcoming of their model by adding not only the cost of lost sales but also the non-constant purchase cost.     

Deterministic inventory model for deteriorating items with capacity constraint and time-proportional backlogging rate

In this paper, a deterministic inventory model for deteriorating items with two warehouses is developed. A rented warehouse is used when the ordering quantity exceeds the limited capacity of the owned warehouse, and it is assumed that deterioration rates of items in the two warehouses may be different. In addition, we allow for shortages in the owned warehouse and assume that the backlogging demand rate is dependent on the duration of the stockout. We obtain the condition when to rent the warehouse and provide simple solution procedures for finding the maximum total profit per unit time. Further, we use a numerical example to illustrate the model and conclude the paper with suggestions for possible future research.     

Characterizations of iron-rich clay modified electrodes and their applications in optical recognition

Optical recognition was studied with modified electrodes based on iron-rich clays. According to energy-dispersive X-ray spectroscopy (EDX), several clay minerals including montmorillonite K10 (mont. K10) contain a lot of iron. Cyclic voltammetry suggested that electrochemically active iron species exist in most iron-rich clays and are likely to reside at different sites. The associated electrochemical activity is strongly pH-dependent and photosensitive. Under UV irradiation (λ ≤ 420 nm), these iron species were activated, and a pronounced photocurrent resulted. When these electrodes were flow-injected with 2-pyridylcarboxylic acids (λ_ab,max = 260 nm), the originally monotonic photocurrent could be modulated into a more recognizable a.c. pattern and the 260 nm optical signal became distinguishable. The photoresponse was highly reproducible, and the response time (t₉₀) was less than 10s.     

多属性决策的组合赋权法

鉴于多属性决策问题中主观赋权法和客观赋权法各有其自身固有的特点，本文依据优化理论提出一种集成方法确定属性权重，该方法既充分利用客观信息，又反映决策者的主观偏好，从而使确定的属性权重更加合理、实用．     

Structure of Cytochromec and Its Platinum-modified Derivatives by Fourier Transform Infrared Spectroscopy

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新重丰中子同位素239Pa

用50MeV/u ¹⁸O离子同天然铀靶反应产生了新重丰中子同位素²³⁹Pa.用放射化学法从反应产物中分离Pa活性,通过观测²³⁹Pa及子体²³⁹U衰变所得到的结果显示:首次合成和鉴别了新重丰中子核素²³⁹Pa,并测定出²³⁹Pa的半衰期为106±30min.