11—溴代十一酸的合臧琛

11－溴代十一酸是尼龙－11单体的中间体，以10－十一烯酸和溴化氢为原料合成11－溴代十一酸，通过实验得出溴代反应的最佳工艺条件为：引发剂用量2％，溴代温度0－15℃，反应时间1h，溶剂为甲苯，10－十一烯酸与甲苯的最佳配比20％，上述条件下，溴代反应的收率达92％以上。     

杀菌剂5—氯—2—甲基—3—异噻唑酮的合成

通过三步反应合成５－氯－２－甲基－３－异噻只酮。ａ）丙烯酸甲酯、多硫化钠、亚硫酸钠在０℃～５℃反应５ｈ得二硫代丙烯酸甲酯,收率９０％;ｂ）二硫代丙烯酸甲酯、甲苯、甲醇混合液在１５℃～２０℃下滴加甲胺反应１０ｈ得Ｎ,Ｎ－二甲基０－二硫代丙烯酰胺,收率１００％;ｃ）Ｎ,Ｎ－二甲基－二硫代丙烯酰胺、二氯乙烷混合液在２５℃滴加二氯砜升温反应１５ｈ,经过后处理得５－氯－２－甲基－３－异噻唑酮。     

5—甲基—2—氨基—1，3，4—噻二唑的合成

本文报道了用硫代氨基脲与乙酸在盐酸、磷酸、多聚磷酸、硫酸等催化下，合成5－甲基－2－氨基－1，3，4－噻二唑，并对工艺条件进行了实验。结果表明，最佳工艺条件为硫代氨基脲与乙酸的摩尔比为1：1．4，浓盐酸催化，回流3小时，产率为74．34％。     

4-氨基吡啶的合成工艺进展

分别介绍了以异烟酸为原料经酯化、酰胺化、霍夫曼降解反应合成4－氨基吡啶；以吡啶为原料，经氧化，硝化，铁－酸还原或催化加氢合成4－氨基吡啶及其他合成4－氨基吡啶的路线，并对这些路线进行了探讨。     

3-(2-氯苯基)-5-甲基-4-异唑甲酸的合成研究

以邻氯苯甲醛、羟胺和乙酰乙酸乙酯为主要原料，经过肟化、氯代、环合和水解反应，合成了氯唑青霉素中间体———３－（２－氯苯基）－５－甲基－４－甲基异唑甲酸。总收率达５０％以上。     

光敏剂N-丁基-2-乙氧基硫代吖啶酮的合成

以邻氯苯甲酸和对乙氧基苯胺为原料，经过胺的苯基化、二芳胺的环化、N－烷基化、硫代化反应合成了N－丁基－2－乙氧基硫代吖啶酮。各步中间产物和目标产物的结构均经红外光谱和质谱确认，通过正交设计实验，得出环化反应的最佳反应条件：温度为100℃，时间为30min，浓硫酸为2－羧基－4′－乙氧基二苯胺的配比为5：1（mL/g)，在此条件下反应收率达78．6％。N－丁基－2－乙氧基硫代吖啶酮的光吸收可延伸到540 nm，在可见光区的最大吸收峰为503nm.     

化学杂交剂氧代烟酸的合成

以4－羟基－6－甲基－2－吡喃酮和对氯苯甲酰氯为起始原料，经过缩合、转位、酯化等五步反应，制得氧代烟酸，五步总收率37．6％。     

1－溴－4－溴甲基苯的简易合成及应用

以对溴甲苯为原料，Ｎ－溴代丁二酰亚胺为溴化剂，利用光引发的自由基反应合成了１－溴－４－溴甲基苯，产率可达８０％，并利用它制得了一个新的有机金属前体。     

β—棕榈酰氨基乙醇异烟酸酯的合成

以棕榈酸为起始原料，合成了具有强抗炎活性的β-棕榈酰氨基乙醇异烟酸酯，合成路线简捷，操作简便，反应条件温和，原料易得，总收率（以棕榈酸计）可达77％。     

4，4’－硫代双［2－（1，1－二甲基乙基）－5－甲基苯酚］的合成及鉴定

报道了４，４′－硫代双［２－（１，１－二甲基乙基）－５一甲基苯酚］的合成方法及结构鉴定。     

Alkylation of Staurosporine to Derive a Kinase Probe for Fluorescence Applications

The natural product staurosporine is a high‐affinity inhibitor of nearly all mammalian protein kinases. The labelling of staurosporine has proven effective as a means of generating protein kinase research tools. Most tools have been generated by acylation of the 4′‐methylamine of the sugar moiety of staurosporine. Herein we describe the alkylation of this group as a first step to generate a fluorescently labelled staurosporine. Following alkylation, a polyethylene glycol linker was installed, allowing subsequent attachment of fluorescein. We report that this fluorescein–staurosporine conjugate binds to cAMP‐dependent protein kinase in the nanomolar range. Furthermore, its binding can be antagonised with unmodified staurosporine as well as ATP, indicating it targets the ATP binding site in a similar fashion to native staurosporine. This reagent has potential application as a screening tool for protein kinases of interest.     

SPA方法快速检验食品志贺氏菌的研究

ＳＰＡ（ＳｔａｐｈｙｌｏｃｏｃｃａｌＰｒｏｔｅｉｎＡ）是某些金黄色葡萄球菌细胞壁的一种蛋白质成分,具有同人和多种哺乳动物ＩｇＧ分子Ｆｃ段结合的能力。本方法用含Ａ蛋白丰富的金黄色葡萄球菌菌体与志贺氏菌属抗血清在一定条件下混合致敏,让抗体结合到金黄色葡萄球菌细胞壁Ａ蛋白上,制成ＳＰＡ诊断试剂。样品经过增菌后,即可用ＳＰＡ诊断试剂来检验。由于金黄色葡萄球菌表面丰富的Ａ蛋白能结合大量抗体,大大提高了检验方法的敏感性,缩短了检验周期     

Ligand-Directed Chemistry on Glycoside Hydrolases – A Proof of Concept Study

Selective covalent labelling of enzymes using small molecule probes has advanced the scopes of protein profiling. The covalent bond formation to a specific target is the key step of activity-based protein profiling (ABPP), a method which has become an indispensable tool for measuring enzyme activity in complex matrices. With respect to carbohydrate processing enzymes, strategies for ABPP so far involve labelling the active site of the enzyme, which results in permanent loss of activity. Here, we report in a proof of concept study the use of ligand-directed chemistry (LDC) for labelling glycoside hydrolases near – but not in – the active site. During the labelling process, the competitive inhibitor is cleaved from the probe, departs the active site and the enzyme maintains its catalytic activity. To this end, we designed a building block synthetic concept for small molecule probes containing iminosugar-based reversible inhibitors for labelling of two model β-glucosidases. The results indicate that the LDC approach can be adaptable for covalent proximity labelling of glycoside hydrolases.     

Composition Analysis of Free Fatty Acids from <Emphasis Type="Italic">Swertia</Emphasis> Species by a Novel Pre-column Fluorescence Labelling Method Using HPLC-FLD

Free fatty acids (FFA) are basic and indispensable components of medicinal plants. Many researches indicate that the efficacy of medicinal plant requires the presence of FFA. In the present study, ultrasonic-assisted extraction of FFA from Swertia species was optimized by response surface methodology (RSM), ensuring the highest FFA recoveries. A novel pre-column fluorescence labelling method using 2-(5-benzoacridine)ethyl-p-toluenesulfonate (BAETS) as a labelling reagent has been developed for highly sensitive and selective analysis of FFA by HPLC with fluorescent detection (FLD) and online mass spectrometry identification. RSM was also employed to optimize the fluorescence labelling of FFA. HPLC separation of 17 FFA derivatives was carried out on a reversed-phase Hypersil BDS C₈ column (4.6 × 200 mm, 5 μm, Agilent Co.) with a gradient elution. The detection limits and quantifications were as low as 0.60 and 1.22 ng mL⁻¹, respectively. FFA analysis from nine Swertia species was performed by the newly developed method, and the FFA composition of these Swertia samples was first reported.     

DABS-Cl 试剂在反相高效液相色谱中的应用

选定了两套完全不同的色谱条件,并对 DABS-氨基酸进行了高效液相色谱分析实验。DABS-Cl 与氨基酸的衍生反应所需的时间不足 lh。     

Characterisation of Photoaffinity‐Based Chemical Probes by Fluorescence Imaging and Native‐State Mass Spectrometry

Chemical probes are small‐molecule reagents used by researchers for labelling and detection of biomolecules. We present the design, synthesis, and characterisation of a panel of 11 structurally diverse photoaffinity labelling (PAL) probes as research tools for labelling the model enzyme carbonic anhydrase (CA) in challenging environments, including in protein mixtures and cell lysates. We targeted the ubiquitous CA II as well as the two cancer‐associated CAs (CA IX and CA XII) that are of high priority as potential biomarkers of aggressive and/or multidrug‐resistant cancer. We utilise an atypical biophysical approach, native state mass spectrometry, to monitor the initial protein–probe binding and subsequent UV crosslinking efficiency of the protein:probe complex. This mass spectrometry methodology represents a new approach for chemical probe optimisation and development that might have broader applications to chemical probe characterisation beyond this study. This also represents one of the first studies, to the best of our knowledge, in which a comprehensive set of PAL probes has been used to establish the relationship between probe structure, noncovalent protein–probe binding, and covalent protein–probe crosslinking efficiency. Our results demonstrate the benefits of a comprehensive analysis of chemical probe structure–activity relationships to support the development of optimum chemical probes.     

Polymeric nanomicelles for cancer theragnostics

Recently, interdisciplinary research in cancer diagnosis and therapy has evolved to the point where nanotechnology particularly polymeric nanodelivery systems are utilized for theragnostic applications. Nanoscale are being trialed for specific targeted delivery of drugs, micelles, antibody, DNA, protein, etc. to cancer sites to improve the therapeutic efficacy due to improved distribution specificity, increased internalization, and intracellular drug delivery that minimize the side effects. Polymeric micelles have been subjected to extensive studies in the field of drug delivery, functioning as drug solubilizers and carriers. More recently, a micelle constructed as a hybrid from hydrophilic oligonucleotide and hydrophobic polymer has drawn close attention. Mostly used micelles are synthesized with polymer and have several physical properties, including molecular weight and copolymer block composition, which can be tailored to alter the vesicle structure. In this review, we focused on the different polymeric nanodelivery systems is association with different type of cancer therapeutics such as micelles, drug, aptamer, DNA, recombinant protein, miRNA, siRNA, small inhibitors, gene, antibody, proteins and some conjugating molecules that involved in cancer therapy have been discussed.     

Rheology and machining performance of waterborne biopolymer labelling adhesives

Machining performance is one of the most important features of waterborne biopolymer labelling adhesives. Various deformation processes on the labelling machine have been analysed in relation to the rheology characteristics of adhesive materials. It has been shown that satisfactory machining performance requires adhesive materials to have particular properties under both shear and extensional deformations. Flow behaviours of commercial labelling adhesive products were tested over a very wide range of shear rate. Time dependences of the apparent shear viscosity were examined at selected shear rates. An adhesive with a smooth flow behaviour and only slight time dependence tends to perform better on the labelling machine. Results found in this work can be used as guide for rheology assessment in the development of new waterborne biopolymer adhesives.     

Label-free impedimetric immunosensor for sensitive detection of atrazine

Impedance spectroscopy transduction combined with the immunosensor technology has been used for the determination of atrazine, a herbicide The sensor electrode was based on the immobilization of anti-atrazine antibody by affinity binding onto a polypyrrole film N-substituted by nitrilotriacetic acid NTA electrogenerated on a gold electrode. The poly NTA film was previously modified by the coordination of Cu2 ions by the chelating NTA centers. The anti-atrazine antibody Fab fragment K47 modified with histidine-tag was then anchored by affinity interactions between the histidine-tag and the coordinated Cu2. Cyclic voltammetry experiments confirm that the antibody immobilization and the resulting immunosensor were applied to the impedimetric detection of atrazine without reagent and labelling step. The immunoreaction of atrazine on the attached anti-atrazine antibody directly triggers an increase in the charge transfer resistance proportional to the atrazine concentration, allowing the detection of extremely low atrazine concentration, namely 10 pg mL⁻¹.     

Protein determination by nuclear magnetic resonance

Protein may be determined using a pulsed nuclear magnetic reso-nance (NMR) spectrometer in conjunction with a relaxation reagent. These reagents exhibit characteristic nuclear relaxation rates, controlled by a paramagnetic ingredient such as copper, and these rates are altered if substances are added which can bind the copper. The method is fast and simple. Sample and reagent are mixed, brought to a standard temperature and transferred to the spectrom-eter for measurement. Sample throughput can be high since the time for the spectrometer reading is on the order of 30 sec. Compositions and methods of use are given for 2 copper-based reagents together with the results on a number of materials. The alkaline copper reagent gives a very similar response to different types of protein and it appears suitable for meat, fish and for other protein materials low in carbohydrates. It shows a response to carbohydrate which depends strongly on type. The acid copper reagent is intended for measurements of vegetable or seed protein and similar applications where carbohydrate is present. This reagent does not respond to carbohydrates tested; the response to protein depends on the type of protein.