Design,Synthesis and Herbicidal Activity of Novel Sulfonylureas Containing Tetrahydrophthalimide Substructure

To develop novel sulfonylurea herbicides, a series of chlorsulfuron derivatives was designed and synthesized through introducing tetrahydrophthalimide substructure taken from protoporphyrinogen IX oxidase(PPO) inhibitors onto the critical 5-position of the classical benzene ring. The structures of title compounds were confirmed by infrared spectroscopy, ultraviolet spectroscopy, ¹H and ¹³C NMR spectrometry, mass spectrometry and elemental analysis. In addition, the crystal structure of compound II-5 was further determined by X-ray diffraction analysis. Bioassay results showed that individual compounds exhibited good herbicidal activities, especially compound II-8, which displayed 100% inhibition rate against Echinochloa crusgalli at 150 g/ha(1 ha=10⁴ m²) with the method of foliage spray in the pot experiment.     

An Enzyme Immunoassay for the Determination of Methabenzthiazuron

Abstract

A sensitive enzyme immunoassay is described for the determination of the urea herbicide methabenzthiazuron. The assay is carried out with polyclonal antibodies, which were raised in rabbits by immunization with a methabenzthiazuron-BSA conjugate containing five methabenzthiazuron residues per molecule. The ELISA was optimized on microtiter plates with a peroxidase-methabenzthiazuron tracer. The middle of the test (50% B/B₀) was found at 1.0 μg/l. The lower detection limit of methabenzthiazuron is c. 0.05 μg/l. Samples can be measured up to 10 μg/l methabenzthiazuron (upper detection limit). The assay does not require concentration or clean-up steps for drinking or ground water samples. Validation experiments showed a good accuracy and precision. Work with monoclonal antibodies is in progress.     

凝胶渗透色谱-气相色谱质谱法测定：花生中6种除草剂农药残留

建立了凝胶渗透色谱一气相色谱质谱（GPC～GC=MS）法测定花生中6种除草剂（氟乐灵、异恶草酮、甲草胺、二甲戊乐灵、乙氧氟草醚、喹禾灵）农药残留的方法。样品经乙腈提取,氨基固相萃取柱和凝胶渗透色谱净化,在选择离子扫描（SIM）模式下进行气相色谱质谱法测定,外标法定量。6种除草剂浓度在0．02-1．00mg／L范围内与色谱峰面积呈良好的线性,线性相关系数为O．9949～0．9998,添加回收率为77．8％-101．6％,测定结果的相对标准偏差为4．4％～11．4％（月=5）,方法的检出限为0．1～1．3μg／kg。     

固相萃取-高效液相色谱法同时检测大米中12种磺酰脲类除草剂的残留

建立了固相萃取前处理净化技术-高效液相色谱（HPLC）同时检测大米中12种磺酰脲类除草剂残留的方法。采用ENVITM-18(C18)硅胶柱和ENVI-Carb(GCB)石墨化碳柱对样品进行净化、萃取,采用C8柱,以乙腈和5 mmol/L 冰乙酸混合溶剂为流动相进行梯度洗脱,在240 nm下进行检测。12种磺酰脲类除草剂在0.01~0.50 μg/g添加范围内的回收率为72.2%~106.5%,相对标准偏差为0.6%~6.4%,检出限为0.01~0.02 μg/g。     

新磺酰脲类化合物的合成及除草活性

新磺酰脲类化合物的合成及除草活性;嘧啶;合成;除草剂     

基于酸性离子液体填充注射器的泡腾辅助微萃取法测定果汁样品中三嗪类除草剂

开发了一种高效、 环保的基于酸性离子液体填充注射器的泡腾辅助微萃取法, 用于测定果汁样品中三嗪类除草剂. 萃取分散采用酸性离子液体[C₄mim][HSO₄], 它对三嗪类除草剂具有较高的溶解度, 其酸性可与碳酸盐反应产生二氧化碳, 从而加速萃取过程. 该实验的提取和分离步骤在注射器中完成, 整个预处理过程完全不需要任何设备辅助. 对碳酸氢钠用量、 酸性离子液体用量、 盐添加量及洗脱溶剂体积等影响萃取效率的实验条件进行了优化. 在最佳条件下, 三嗪类除草剂浓度在1~200 ng/mL范围内获得了良好的线性关系, 相关系数大于0.9984; 检出限(LOD)和定量限(LOQ)分别为0.06~0.18和0.21~0.61 ng/mL, 日间及日内精密度低于8.3%. 实验结果表明, 该方法可用于果汁样品中三嗪类除草剂的测定.     

稠杂环化合物的研究——Ⅵ.3-(3′-吡啶基)-6-脂肪基/芳香基均三唑并[3,4-b]-1,3,4-噻二唑的合成及生物活性研究

本文研究了3-(3′-吡啶基)-4-氨基-5-巯基-1,2,4-三唑在POCl_3存在下与脂肪酸和芳香酸的缩合反应,制得24种新的3-(3′-吡啶基)-6-脂肪基/芳基均三唑并[3,4-b]-1,3,4-噻二唑,利用元素分析、IR、~1H NMR及MS方法确认了结构。部分化合物进行了抗菌和除草试验。     

1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物的合成与生物活性

为寻求高效低毒的农药,设计、合成了一系列新的1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物3a～3j和4a～4d.元素分析,1H NMR,IR和MS证实了它们的结构.初步的生物活性测试结果表明,在10 mg/L浓度下,化合物3a～3j和4a～4d对油菜的根茎均有很好的抑制作用,对油菜的根的抑制率为90.0%～98.7%;于100 mg/L浓度下,对稗草的根抑制率为84.0%～100%.     

精喹禾灵中间体6-氯-2-喹喔啉醇的合成

综述了6-氯-2-喹喔啉醇的合成方法以及国内外研究动态和进展，参考文献20篇。6-氯-2-喹喔啉醇是-种重要的有机化工原料，是合成新型高效除草剂精喹禾灵原药的重要中间体，其合成一般通过6-氯-2-喹喔啉醇-4-氧化物的选择性还原来制取。     

New multiresidue analytical method dedicated to trace level measurement of brominated flame retardants in human biological matrices

A new method has been developed for the multi-residue measurement of the main brominated flame retardants (alpha- and gamma-hexabromocyclododecane (HBCD), tetrabromobisphenol A (TBBP-A) and polybrominated diphenyl ethers including decabromodiphenyl ether) in human biological matrices (serum, adipose tissue and breast milk). The proposed sample preparation procedure focused on reduced solvent and consumable consumption and associated procedural contamination, as well as reduced sample size. This protocol was fully validated and was proved to be suitable for identification of brominated flame retardant residues at ultra-trace level, as attested by preliminary results on real samples.