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。     

超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留

目的建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定畜禽肉组织中17种磺胺类药物残留的方法。方法样品经乙腈提取、浓缩,正己烷脱脂后在正离子模式下以电喷雾电离串联质谱进行测定,外标法定量。结果 17种磺胺类药物在5μg/L~100μg/L范围内线性良好,相关系数0.99,方法检出限为2μg/kg,定量限为5μg/kg。在10、20、100μg/kg的添加水平下,17种磺胺类药物的平均回收率在84.0%~114.2%之间,相对标准偏差(relative standard deviation,RSD,n=6)在0.59%~7.96%之间。结论本方法快速、准确、灵敏,可应用于畜禽肉中17种磺胺类药物残留的同时检测。     

Tribological performance of sulfonamide derivatives as lubricating oil additives in the diester

The load‐carrying capacity, anti‐wear and friction reduction properties of two sulfonamide derivatives added to a synthetic lubricant (diester) were evaluated using a four‐ball test machine. The results indicate that both additives possess good load‐carrying capacities and excellent anti‐wear and friction reduction properties. The surface topography of the rubbed surface was investigated by scanning electron microscopy, and the chemical nature of the anti‐wear films generated on the steel counter‐face was investigated by X‐ray photoelectron spectroscopy. Surface analysis results show that a stable lubricating film consisting of the reaction layer and adsorption layer was formed on the worn surface. Copyright © 2006 John Wiley & Sons, Ltd.     

甲基磺酰胺合成研究

采用二甲基二硫为主要原料 ,经氯化、氨化合成甲基磺酰胺 ,提高了产品收率 ,纯度达 98%以上     

Primary Mode of Action of the Novel Sulfonamide Fungicide against Botrytis cinerea and Field Control Effect on Tomato Gray Mold

Botrytis cinerea is considered an important plant pathogen and is responsible for significant crop yield losses. With the frequent application of commercial fungicides, B. cinerea has developed resistance to many frequently used fungicides. Therefore, it is necessary to develop new kinds of fungicides with high activity and new modes of action to solve the increasingly serious problem of resistance. During our screening of fungicide candidates, one novel sulfonamide compound, N-(2-trifluoromethyl-4-chlorphenyl)-2-oxocyclohexyl sulfonamide (L13), has been found to exhibit good fungicidal activity against B. cinerea. In this work, the mode of action of L13 against B. cinerea and the field control effect on tomato gray mold was studied. L13 had good control against B. cinerea resistant to carbendazim, diethofencarb, and iprodione commercial fungicides in the pot culture experiments. SEM and TEM observations revealed that L13 could cause obvious morphological and cytological changes to B. cinerea, including excessive branching, irregular ramification or abnormal configuration, and the decomposition of cell wall and vacuole. L13 induced more significant electrolyte leakage from hyphae than procymidone as a positive control. L13 had only a minor effect on the oxygen consumption of intact mycelia, with 2.15% inhibition at 50 μg/mL. In two locations over 2 years, the field control effect of L13 against tomato gray mold reached 83% at a rate of 450 g ai ha⁻¹, better than the commercial fungicide of iprodione. Moreover, toxicological tests demonstrated the low toxicological effect of L13. This research seeks to provide technical support and theoretical guidance for L13 to become a real commercial fungicide.     

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.     

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.     

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。     

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.