螺螨酯类似物AC-101的合成与杀螨活性

为寻求高活性的杀螨剂,通过对螺螨酯进行结构改造,合成了新杀螨活性化合物3-(2,4-二氯苯基)-2-氧-1-氧杂螺[4.5]癸-3-烯-4-基-丁基-1-磺酸酯(试验代号:AC-101;暂命名:螺螨丁酯),并开发了24%悬浮剂(SC)和24%可分散油悬浮剂(OD)制剂。室内生物活性测试显示:在1 mg/L质量浓度下,螺螨丁酯对朱砂叶螨螨卵的防效达95%。田间药效试验显示:24%螺螨丁酯SC和OD药后14 d对山楂叶螨的最高防效分别为95.7%和96.2%,药后21 d对山楂叶螨的防效在73.6%以上。螺螨丁酯具有杀螨活性高、速效性好和持效期长的特点,有一定的应用开发价值。     

二丁基一氯化锡杂环羧酸酯的合成与表征

合成了８个新的二丁基一氯化锡杂环羧酸酯。利用元素分析、红外光谱及核磁共振氢谱表征了这些化合物的组成和结构。     

N-亚甲基磷酸壳聚糖有机锡酯的合成、表征及杀螺活性研究

用磷酸和甲醛在稀醋酸介质中对壳聚糖(CTS)进行N-亚甲基磷酸化改性,得到N-亚甲基磷酸壳聚糖(MPCS),用自制的MPCS在苯或甲苯介质中与有机锡发生反应,合成了3个新的N-亚甲基磷酸壳聚糖有机锡酯化合物:MPCS-SnPh3、MPCS-Sn(PhCH2)3、MPCS-SnBu3。通过IR、13C NMR、TG/DTA和X-ray对其结构和性质进行了表征和测试。杀钉螺实验结果表明,当其浓度在1.00 mg/L以上时,浸杀48 h后,钉螺的死亡率达100%。     

三丁基锡氮杂环羧酸酯的合成及应用研究

以三丁基氯化锡和氮杂环羧酸盐为原料,合成了５种新型杀菌剂三丁基锡氮杂环羧酸酯（ｎ Ｃ４Ｈ９）３ＳｎＯ２ＣＲ（Ｒ＝吡啶基,吲哚烷基）,所有产品收率均大于８５％。实验确定了较佳反应条件：三丁基氯化锡和氮杂环羧酸盐的摩尔比为１１．２,反应时间为５ｈ,反应温度为回流温度。样品经元素分析、红外光谱和核磁共振氢谱检测与目标化合物一致。对化合物进行了应用试验,结果表明,在质量分数为０．００５％时,这些化合物的杀菌活性为８８％～１００％。     

含硅二烃基锡二吡啶羧酸酯的合成与结构表征

采用含硅二烃基锡氧化物和相应的吡啶甲酸,合成了7个新的含硅二烃基锡配合物--标题化合物;通过IR、1HNMR、13CNMR和元素分析对它们的结构进行表征.生物活性测定的初步结果表明,目标化合物环已基(三甲基硅基亚甲基)锡二(2-吡啶羧酸酯)Cy(Me3SiCH2)Sn(OCOC5H4N-o)2对肺癌细胞A549和肠癌细...     

辛硫磷类似物的合成及杀螺活性

为寻找新的高效、低毒灭螺药,以取代苯乙腈为原料,经成肟、硫代磷酰化等反应,制得9个辛硫磷类似物(2a～2i),其结构经元素分析、IR、1H NMR和MS确证.初步杀螺筛选结果表明:化合物2a、2b、2h具有显著的杀螺活性,其半数致死浓度LC50值分别为0.31、0.33、0.38 mg/L.     

丁基(三甲基硅基亚甲基)锡二芳香酸酯的合成与结构表征

采用丁基(三甲基硅基亚甲基)二氯化锡和芳香酸,在三乙胺存在下,以1:2的物质的量比进行反应,合成了9个新的混合含硅二烃基锡化合物--标题化合物.通过IR、1HNMR和13CNMR对它们的结构进行了表征.生物活性测定的初步结果表明,目标化合物Bu(Me3SiCH2)Sn(OCOC6H4NO2-p)2对肺腺癌细胞A549有较好的体外抗癌活性.     

三苯基锡(Ⅳ)四氢吡咯荒酸酯的合成、表征、性质及晶体结构

用三苯基氯化锡和四氢吡咯荒酸钠反应 ,合成了三苯基锡 ( )四氢吡咯荒酸酯。通过元素分析、红外光谱和氢核磁共振谱对其结构进行了表征。用 X-射线单晶衍射测定了该化合物的晶体结构。结果表明 ,化合物中锡原子呈五配位畸变三角双锥构型     

嘧螨酯的合成与杀螨活性

以氰胺和异丙醇制备异丙氧基脒甲烷磺酸盐,再与三氟乙酰乙酸乙酯反应制得2-异丙氧基-4-羟基-6-三氟甲基嘧啶,最后与(E)-2-12-(氯甲基)苯基]3-甲氧基丙烯酸甲酯反应合成目标产物嘧螨酯,其结构经核磁、红外验证.生物活性测定结果表明该化合物具有良好的杀螨活性.     

Preparation of water‐soluble chitosan derivatives and their antibacterial activity

Carboxymethyl chitosan sodium (CMCTS) was synthesized by chitosan and chloroacetic acid under an alkali catalyst. Acrylic acid sodium salt and methylacrylic acid sodium salt were grafted onto CMCTS to obtain copolymers with good water solubility. The graft reaction was carried out at 70°C for 2 h, and ammonium persulfate was used as an initiator. The structure changes of chitosan and its derivatives were investigated by the FTIR. The antibacterial activity of chitosan derivatives against Staphylococcus aureus and Escherichia coli were explored by the viable cell counting method. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 1357–1361, 2002     

Synthesis and Characterization of Carboxymethyl Chitosan Grafted Methacrylic Acid Initiated by Ceric Ammonium Nitrate

O-carboxymethyl chitosan (CMCH) was prepared and characterized by FTIR spectroscopy and X-ray diffraction. Grafting of methacrylic acid (MA) onto CMCH using ceric ammonium nitrate (CAN) as an initiator was carried out under nitrogen atmosphere in aqueous solution. Evidence of grafting was confirmed by comparison of FTIR spectra of CMCH and the grafted copolymer as well as scanning electron micrograph (SEM) and X-ray diffraction of the products. The effects of concentration of CAN, MA, reaction time and temperature on graft copolymerization were studied by determining the grafting percentage and grafting efficiency. Keeping other conditions constant, the optimum grafting conditions were obtained as follows: CMCH = 2 gm, CAN = 0.2 M and MAA = 0.581 mol/L, reaction temperature = 40°C and reaction time = 4.5 hr.     

Preparation, characterization and antimicrobial activity of quaternized carboxymethyl chitosan and application as pulp-cap

Quaternized carboxymethyl chitosan (QCMC) was prepared from which carboxymethyl chitosan (CMC) was prepared from chitosan first, then N-quaternary ammonium group was introduced by the reaction of CMC with 2, 3-epoxypropyl trimethylammonium. The structures of the derivatives were characterized by FT-IR, XRD, ¹³C NMR, ¹H NMR and gel permeation chromatography. In vitro antimicrobial activities of QCMC were evaluated against Escherichia coli, which is a Gram-negative bacterium, and Staphylococcus aureus, which is a Gram-positive bacterium. In compared with carboxymethyl chitosan (CMC) and quarternary chitosan (QC) of the same degree of substitusion (DS), we found that QCMC has stronger antimicrobial activity. Then we went deep into study of the relationship between their structure and antimicrobial activity, found that the DS of CMC do little effect to their antimicrobial activity, but as the increase of their DS of quaternization or the decrease of their molecular weight, the antimicrobial activity of QCMC become stronger. QCMC was complexed with calcium hydroxide as pulp-cap. Animal experiment results indicated that QCMC can strongly induce reparative dentine formation and showed a better ability in dentin inducing compared with calcium hydroxide.     

壳聚糖/羧甲基壳聚糖及其衍生物在日化方面的应用

壳聚糖及其衍生物含有大量的氨基和羟基,为壳聚糖的改性或者接枝反应提供了活性基团,壳聚糖/羧甲基壳聚糖因特殊的化学结构而使其具有优异的化学性质,如良好的生物相容性、无毒、生物可降解性以及抗微生物活性等性质,因此受到生物工程、医药、食品、化妆品以及其他一些领域的广泛关注,成为近年来研究开发的热点。对壳聚糖/羧甲基壳聚糖及其衍生物在日用化学中的应用进行了综述,并对其发展趋势进行了展望。     

壳聚糖/N-乙烯基吡咯烷酮接枝共聚物的制备及其性能

以壳聚糖（CS）和N-乙烯基吡咯烷酮（NVP）为原料,本文采用过氧化氢和抗坏血酸共引发剂引发,制备壳聚糖/N-乙烯基吡咯烷酮的接枝共聚物（CS-g-NVP）,研究了引发剂配比、反应温度和反应时间等因素对接枝共聚反应的影响。通过红外光谱、核磁共振和热重分析等对产物进行表征,并考察其吸湿性和亲水性能。结果表明,接枝共聚反应的最佳条件为：引发剂抗坏血酸/过氧化氢的摩尔比为1∶1、反应温度60℃、反应时间12h。接枝共聚产物的吸湿性优于壳聚糖,在饱和氯化钙和饱和硫酸铵环境下产物的吸湿率分别为3.68%和23.1%,高于原料壳聚糖的0.41%和9.77%,产物具有良好的亲水性和水溶性,能溶解于酸性和碱性水溶液中。     

Antibacterial activity of cationically modified cotton fabric with carboxymethyl chitosan

A water‐soluble carboxymethyl chitosan was prepared with a view to develop a multifunctional finish on cotton. Carboxymethyl chitosan (CMCTS) was synthesized by chemical reaction of chitosan with monochloroacetic acid under alkaline condition. The water soluble CMCTS was applied to cationized cotton with different concentrations. The treated fabrics were characterized through monitoring the textile physical properties and for the antibacterial activity against Escherichia coli DSMZ 498 and Micrococcus luteus ATCC 9341. The results obtained show that the physical properties of the treated fabrics are improved by increasing the CMCTS concentration, as well as the antibacterial activity. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Hemocompatibility evaluation of polyurethane film with surface‐grafted poly(ethylene glycol) and carboxymethyl‐chitosan

To improve the hemocompatibility and biocompatibility of polyurethanes (PUs), PU surface was firstly modified by poly(ethylene glycol) PEG through acryloyl chloride and subsequently grafted on carboxymethyl‐chitosan (CMCS). Attenuated total reflection Fourier transform infrared spectroscopy and X‐ray photoelectron spectroscopy analysis confirmed that carboxyl‐chitosan was grafted onto PUs surface. The surface properties of unmodified and modified PU films were determined and compared by water contact angle assessment. After PEG and CMCS grafting, the surface energy of the PU film was increased. Furthermore, the hemocompatibility of the modified PU films was systematically evaluated by bovine serum albumin (BSA) adsorption, the dynamic blood clotting test, the platelet adhesion test, and the hemolytic test. It appears that BSA adsorption and platelet adhesion were significantly curtailed for the modified PU films. Therefore, the obtained results showed the modified PU film has better hemocompatibility. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

阳离子型壳聚糖接枝共聚物的制备及其絮凝性能研究

以壳聚糖(Cts)、丙烯酰胺(AM)、二甲基二烯丙基氯化铵(DMDAAC)为原料,过硫酸铵为引发剂,合成了阳离子型壳聚糖三元接枝共聚物.最佳的合成条件为:反应温度50℃,引发剂浓度6mmol·L-1,Cts:AM为1:3(m/m),AM:DMDAAC为3:3(m/mL),反应时间3h.该条件下接枝共聚物的接枝率、阳离子度分别达287.5%、26.7%.生活废水的絮凝实验表明,接枝共聚物有优异的絮凝能力.与Cts、PAM、PAC比较,接枝共聚物具有用量少,除浊率高等优点.     

双癸基二甲基羧酸铵反离子碳链长度对其表面活性和应用性能的影响

通过对不同反离子碳链长度(n=2,4,6,8,10,12)的双癸基二甲基羧酸铵的表面活性及泡沫性能、乳化性能和润湿性能进行测定,探讨反离子碳链长度对季铵盐表面活性剂的表面活性及应用性能的影响。结果表明:随着反离子碳链长度(n=2,4,6,8,10,12)的增加,双癸基二甲基羧酸铵的表面活性逐渐增强,其临界胶束浓度(cmc)逐渐减小,最低表面张力(γcmc)先降低后升高,当反离子碳链长度n=10时,γcmc达到最低,降低水表面张力20 m N/m的效能(pc20)逐渐增大,饱和吸附量(Гtotal)逐渐增大,单个分子占有面积(Am)逐渐减小;泡沫性能和乳化性能均随着反离子碳链长度的增加先增强后减弱;润湿性能随着反离子碳链长度的增加而逐渐增强。     

Graft copolymerization of hydroxyethyl methacrylate onto chitosan

Chitosan is a polysaccharide derived from chitin, which is commonly found in shellfish waste materials. The present work is concerned with the graft copolymerization of 2-hydroxyethylmethacrylate (HEMA) onto chitosan using thiocarbonation–potassium bromate for redox initiation. The combined effects of the principal reaction variables for the grafting reaction were studied systematically. This grafting reaction was studied with respect to percentages of graft yield (%G.Y.), homopolymer (%H.P.), and total conversion (%T.C.). A tentative polymerization mechanism is proposed. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 683–702, 2001