双胍辛醋酸盐杀菌剂及其两种中间体的合成与生物活性

O-methylisourea acetate was synthesized by two procedures from the main raw materials including carbamide, dimethyl sulfate, acetic acid and concentrated sulfuric acid. Its content reaches 98 % and the total yield attains to 70%. 1, 17-Diamino-9-azaheptadecane was first synthesized by two procedures using sebcic acid, 1,8-octanediamine, sodium azide and concentrated sulfuric acid as the main raw materials. Its content reaches 98% and the total yield is 65%. The structure of both were confirmed by FT-IR, ^1H NMR and their available analysis method was established. Fungicide bis-(8-guanidino-octyl )amine acetate was synthesized from these two intermediates and its structure was confirmed by FT-IR and ^1HNMR. Fungicidal activity test showed that it is a kind of broad-spectrum fungicide with notably effect.     

烯唑醇聚合物杀菌剂的合成和生物活性测试

为了克服烯唑醇易受风、雨水、光及微生物等因素影响而大量流失的缺点,通过化学反应使其与苯乙烯-马来酸酐交替共聚物结合,得到了一种杀菌聚合物。试验结果表明：该聚合物在模拟的应用环境中经水解和微生物降解等过程能够以有效剂量持续释放出具有杀菌性的活性组分,其杀菌活性与烯唑醇基本一致,持效期至少30天。这种烯唑醇高分子缓释剂对于有效利用农药,减少农药戏留,保护环境具有实际意义。     

新型二芳基吡唑衍生物的合成及其抑菌活性

水杨醛与2,4-二氯苯乙酮缩合形成α,β不饱和酮后与水合肼关环形成3-(2,4-二氯苯基)-5-(2-羟基苯基)吡唑(2),2与烷基酰氯反应合成了6个未见文献报道的3-(2,4-二氯苯基)-5-(2-酯基苯基)-4,5-二氢-N-酰基吡唑衍生物(3a～3f),其结构经1HNMR,IR和元素分析表征。对3进行了初步生物活性测试,结果表明3浓度为50mg·L-1时,3f,3d对水稻纹枯菌的抑菌率分别为77.4%,60.3%,对稻瘟病菌的抑菌率分别为66.3%,69.2%;3e对油菜菌核菌抑菌率为79.2%。     

2-甲基-5,7-二氢噻吩并[3,4d]嘧啶6,6-二氧化物的合成新方法

对4-氯-2-甲基-5,7-二氢噻吩并[3,4-d]嘧啶6,6-二氧化物为原料合成2-甲基-5,7二氢噻吩并[3,4-d]嘧啶6,6-二氧化物的方法进行了改进.与文献报道的Pd-C/H2脱氯方法相比,用新的甲苯-锌粉-氢氧化钠溶液-TBAB体系常压脱氯,简便易行,避免了加氢脱氯的危险性,降低了成本,产物收率达92 %.对反应条件进行了优化:甲苯为溶剂,TABA为相转移催化剂,n(4-氯嘧啶二氧化物)∶n(Zn)∶n(NaOH)=1∶10∶20,温度100 ℃,反应时间2 h.     

Fungicidal and spectral studies of some triphenyltin compounds

In the interest of developing a more effective fungicide to combat Dutch elm disease, our laboratories have synthesized several triphenyltin carboxylates and some 1:1 addition compounds of triphenyltin chloride using 2,3-disubstituted thiazolidin-4-ones as the ligand and screened them in vitro against Ceratocystis ulmi, the causative agent of Dutch elm disease, using a shake culture method. Elemental analyses and spectroscopic data indicate that the structures of the carboxy- lates in the solid state are monomeric with a tetrahedral tin atom with the exception of the furan-2-carboxylic acid derivative, which was found to be polymeric. The triphenyltin chloride adducts are trigonal-bipyramidal with the three phenyl groups in the equatorial plane. Far-infrared data indicate that the three phenyl groups are not co-planar. Screening results for both series of organotins indicate that these two classes of compounds are effective inhibitors of Ceratocystis ulmi, with the adducts having a higher activity. The furan-2-carboxylic acid derivative has a markedly decreased activity compared with the other carboxylates and this is attributed to its polymeric structure. © 1998 John Wiley & Sons, Ltd.     

分散固相萃取-液相色谱-串联质谱法测定谷物、蔬菜、水果中27种新型杀菌剂

建立了同时检测谷物、蔬菜和水果中27种新型杀菌剂的分散固相萃取-液相色谱-串联质谱(DSPE-LC-MS/MS)分析方法。样品经1%(体积分数)乙酸丙酮溶液提取,以无水硫酸镁(MgSO_4)脱水,经N-丙基乙二胺(PSA)、C_(18)、无水MgSO_4、多壁碳纳米管(MWCNT)混合净化剂净化,经C_(18)色谱柱分离,用乙腈和体积分数为0.1%的甲酸水溶液(含5 mmol/L乙酸铵)梯度洗脱,多反应监测(MRM)正离子模式扫描,采用外标法定量。噻呋酰胺和氯啶菌酯在20.47~200μg/kg范围内线性关系良好,其他25种新型杀菌剂在0.02~100μg/kg范围内线性关系良好,相关系数R~2≥0.995 0,加标回收率为70.02%~117.6%,相对标准偏差(RSD)为0.01%~19.62%(n=3)。噻呋酰胺和氯啶菌酯的检出限为6.15~16.67μg/kg,定量限为20.47~55.5μg/kg。其他25种新型杀菌剂的检出限为0.006~4.44μg/kg,定量限为0.02~14.79μg/kg。该方法简便、快速、可靠,可用于谷物、蔬菜、水果中27种新型杀菌剂的快速测定。     

化合物2杀菌活性的模糊聚类分析

应用模糊数学聚类分析的方法,分析了化合物2对几种病菌的抑制作用。算法公式数学模型处理得到模糊相似矩阵,进而画出动态聚类分析图即可分析化合物2对几种病菌抑制作用的特点及异同。此分析有很重要的实际应用价值。     

取代嘧啶基硫脲类化合物的合成及生物活性

目的合成新的广谱、高效优良硫脲类杀菌剂。方法以氯甲酸酯与含不同取代基的嘧啶胺为原料,回流反应。结果合成了14个取代嘧啶基硫脲类化合物,其中12个化合物为首次报道的新化合物。结构组成经元素分析、IR及1H NMR确认,并测定了其对5种植物病菌的室内毒力作用。结论合成方法简便、易行,且大部分化合物具有良好的抑菌和杀菌活性。     

超声萃取结合超高效液相色谱法测定皮革中10种防霉剂

建立了皮革样品中10种防霉剂(氨基苯磺酰胺、苯并咪唑、BIT、MBT、IPBC、PCMC、水杨酰苯胺、OPP、TCMTB和OIT)的超高效液相色谱(UPLC)检测方法。样品经甲醇超声萃取,T3色谱柱分离后,甲醇和0.1%甲酸水为流动相梯度洗脱,二极管阵列检测器测定。在优化条件下,10种防霉剂在一定的浓度范围内线性关系良好,相关系数(r~2)均不小于0.999 3,除IPBC的方法定量下限(S/N=10)为190.0 mg/kg外,其余9种防霉剂的方法定量下限为4.0~8.0 mg/kg,平均回收率为81.3%~104.9%,相对标准偏差(RSD,n=6)为4.7%~11.2%。该方法前处理简单、分离效果好,适用于皮革样品中10种防霉剂的同时测定。     

Synthesis and antifungal activity of chitosan-silver nanocomposite synergize fungicide against Phytophthora capsici

Fungicides are important tools for preventing pathogens and maintaining crop quality; however, their effectiveness was directly affected by high-priced, toxicity, and environmental pollution. As a result, it is necessary to get a safe and efficient antimicrobial agent against agricultural pathogens. In this study, silver-incorporated chitosan nanocomposites (Ag@CS) were first prepared in which CS was used as reducing and stabilizing agent and then these nanocomposites was synergized with fungicide Antracol (An), Ag@CS/An, against Phytophthora capsici causing Phytophthora blight in pepper. The obtained nanocomposites were characterized by Fourier transform infrared (FTIR), X-ray diffraction analysis (XRD), thermogravimetric analysis (TGA), dynamic light scattering (DLS), and transmission electron microscopy (TEM). These results showed that Ag@CS and Ag@CS/An were successfully synthesized with spherical shape AgNPs having diameter of 20.3?±?0.7?nm and 44.6?±?0.3?nm, respectively. More importantly, Ag@CS/An was found to have significantly stronger antifungal ability than each component alone, analyzed by agar diffusion method. It might be anticipated that Ag@CS/An has a promising future as nano-antibiotic materials for agriculture.