液相色谱串联质谱法测定鸡蛋粉中16种磺胺类药物的残留量

目的建立液相色谱串联质谱法同时定性定量测定鸡蛋粉中16种磺胺类药物残留量的分析方法。方法样品中的16种磺胺类物质用0.2%甲酸乙腈提取后,由Oasis Prime HLB固相萃取柱净化,经SB C18色谱柱(2.1 mm×150 mm, 3.5μm)分离,以0.1%甲酸溶液和乙腈为流动相进行梯度洗脱,流速为0.25 mL/min,柱温为30℃。多反应监测模式测定,外标法定量。结果 16种目标化合物线性良好,相关系数均大于0.9992,方法的最低检出限在0.1～0.5μg/L之间,大部分待测物的平均回收率为79.9%～95.8%,相对标准偏差为3.1%～12.0%。结论该方法快速、准确,适用于鸡蛋粉中16种磺胺类药物残留量的检测。     

Sulfonamide Inhibitors of β-Catenin Signaling as Anticancer Agents with Different Output on c-MYC

The Wnt/β-catenin pathway is often found deregulated in cancer. The aberrant accumulation of β-catenin in the cell nucleus results in the development of various malignancies. Specific drugs against this signaling pathway for clinical treatments have not been approved yet. Herein we report inhibitors of β-catenin signaling of potential therapeutic value as anticancer agents. Ethyl 4-((4-(trifluoromethyl)phenyl)sulfonamido)benzoate (compound 14 ) inhibits the effect on Wnt reporter with an IC₅₀ value of 7.0 μM, significantly reduces c-MYC levels, inhibits HCT116 colon cancer cell growth (IC₅₀ 20.2 μM), does not violate Lipinski and Veber rules, and shows predicted Caco-2 and MDCK cell permeability P_app>500 nm s⁻¹. Compound 14 seems to have potential for the development of new anticancer therapies.     

Preparation of Dicarboxylic Acid Containing Sulfonamide Based Resin and Removal of Basic Dyes

Polymer and dye interaction leading to polymer-dye complex formation exhibits many interesting and important practical features. For this purpose, dicarboxylic acid containing resin was prepared in two steps starting from poly (styrene-divinyl benzene) (PS-DVB) (10% crosslinking) based beads with a particle size of 400-590 µm, according to the synthetic protocol; chlorosulfonation, sulfamidation with iminodiacetic acid. Dye extraction experiments were carried out by contacting wetted resin samples with aqueous dye solutions at room temperature. Capacities were determined by colorimetric analysis of the residual dye content. Dye sorption capacity of the resin was found to be (0.67-0.63 g g^?1 resin). This material is also able to remove the cationic dyes completely even from highly diluted aqueous dye solutions.     

Preparation of Sulfonamide Containing Cellulose Based Sorbent for Removal of Mercury Ions

A new sulfonamide containing cellulose based sorbent was prepared in three steps; poly (acrylonitrile) (PAN) grafting onto cellulose by redox polymerization method, amination of PAN grafted cellulose with ethylenediamine, and sulfamidation with benzene sulfonyl chloride. The resulting polymeric sorbent, which had a sulfonamide content of 3.4 mmol/g, was effective for the removal of mercury ions from aqueous solutions. The mercury sorption capacity of the sorbent is around 1.95 mmol/g under non-buffered conditions. The experiments performed under identical conditions with some metal ions reveal that Cd(II), Mg (II), Zn(II), and Fe(III) ions are also extractable in low quantity (0.02–0.46 mmol/g). The sorbed mercury can be eluted by repeated treatment with hot acetic acid.     

Synthesis and characterization of fluoropoly(amide–sulfonamide)s via polycondensation

Novel fluorine-containing polymers, fluoropoly(amide–sulfonamide)s were synthesized for the first time by polycondensation from β-hydroxytetrafluoroethanesulfonic acid sultone (TFE-sultone) and hexamethylenediamine. The chemical structures of the obtained F-PASAs were characterized by intrinsic viscosity measurements, GPC, FTIR, ¹H NMR, ¹⁹F NMR and element analysis in detail. Thermal properties and optical property of F-PASAs were investigated by DSC, DMA, TGA and UV–vis spectra, respectively. The investigation indicated that these functional fluoropolymers in which there are both amide and sulfonamide linkages along the polymer main chains possessed distinctive structure as well as unique properties such as thermal properties, clean and high transparency and compatibility with nylons.     

樟脑衍生的手性磺酰胺醇的合成及催化性能

由天然樟脑合成了一个新手性磺酰胺醇,并对其在二乙基锌对苯甲醛的对映选择性加成中的催化性能进行了研究,获得了73%化学产率和9.2%e.e.。     

新手性磺酰胺醇催化二乙基锌对苯甲醛的不对称加成反应

由天然樟脑和(L)-苯丙氨酸合成了4个新的手性磺酰胺醇,并对其在二乙基锌对苯甲醛的不对称加成中的催化性能进行了研究。这4个手性磺酰胺醇表现出中等程度的催化活性和较差的不对称诱导作用。     

硫化促进剂NS的开发研究

在非离子表面活性荆存在下采用微压一步缩合法合成了N-叔丁基-2-苯并噻唑次磺酰胺,并讨论了原料配比、反应温度、反应时间等条件对反应的影响。     

Polymeric decontaminant 2 (N,N‐dichloropolystyrene sulfonamide): Synthesis,characterization, and efficacy against simulant of sulfur mustard

A polymeric decontaminant N,N‐dichloropolystyrene sulfonamide was synthesized by different steps from starting material polystyrene and followed by sulfonation, chlorosulfonation, and amidification. Halogeno‐sulfonamide was obtained by treatment of sodium hypochlorite with sulfonamide resin. It was characterized by FTIR, solubility, viscosity, DSC, and TGA techniques. Efficiency of this polymer as decontaminant was evaluated by reaction with 2‐chloro ethyl phenyl sulfide, a simulant of sulfur mustard (SM) at room temperature. This decontamination reaction was monitored by gas chromatography (GC) and products were identified by gas chromatography‐mass spectrometry (GC‐MS). The positive chlorine content of this polymer was checked by standard iodometry titration. The synthesized positive chlorine compound is observed to be a promising decontaminant against simulant of sulfur mustard, chiefly in the situation where use of aqueous medium such as acetonitrile : water (2 : 1) is precluded. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

甲基磺酰胺的合成研究

本文采用硫酸二甲酯为主要原料经氯化、氨化合成甲基磺酰胺，产品收率可达６６．８％，纯度在９８％以上。