氯氰菊酯农药中杂质及立体异构体的分离、鉴定

本文应用薄层色谱、气相色谱法分离了氯氰菊酯原药中的立体异构体和主要杂质。经GC-MS鉴定,其主要杂质为3-(2,2-二氯乙烯基)2,2-二甲基环丙烷羧酸,3-含氧基苯基安息香醛,3-含氧基苯基安息香醇及3-含氧基甲基偶联苯。它们与该农药在动物和土壤中的主要代谢物相同。     

一种快速测定异丙隆原药中3个FAO杂质的方法

旧的]建立一种反相高效液相色谱法,用于对异丙隆原药中异丙隆邻位异构体、间位异构体及N,N'-双-[3-(1-甲基乙基)苯基]脲含量的分析.[方法]采用Poroshell 120 PFP色谱柱,波长分别为240、256 nm,以乙腈-水作为流动相进行分离,测定异丙隆原药中3个杂质的含量.[结果]该方法中异丙隆邻位异构体、...     

抗蚜威原药及其杂质的GC-MS分析研究

采用气相色谱-质谱联用法对抗蚜威原药进行分离鉴定,使用HP-5MS(30 m×0.25 mm,0.25μm)毛细管柱,EI离子源,得到抗蚜威及其4个杂质的质谱图,根据标准谱库推断出这些谱图对应的杂质成分,根据合成路线探讨了杂质来源可能,并讨论了抗蚜威的质谱裂解规律。     

手性高效液相色谱法测定虫酰肼原药中的异构体杂质

采用高效液相色谱法,使用Chiralcel OD-H手性柱,对虫酰肼原药中主成分与异构体进行了分离,并对异构体杂质进行了定量分析。结果表明,该方法分析异构体杂质的线性相关系数为0.9997,变异系数为0.25%,回收率在98.57%～101.47%之间。     

林丹

1.1 原药本品主要含有1,2,3,4,6,6-六氯环己烷的丙种异构体,为白色或接近白色的细粒,薄片或粉末,不含有外来杂质或添加的改性剂。 1.2 化学及物理的技术条件从出售商品的任一部分取样(见方法WHO/M/1)都应符合1.1节及下面的技术要求:     

杀螟松、乐果及水杨硫磷的热分解及其稳定化方法

<正>有机磷农药特别是有机磷农药的固体制剂如粉剂、可湿粉剂、颗粒剂等的贮存稳定性,是农药生产和使用部门关心的主要问题之一。 影响有机磷农药分解的原因较多,如原药性质、载体性质以及环境条件(水份、温度、光辐射)等等。本文简单介绍几个有机磷农药的热分解机理及其稳定化途径。 日本前田尚良等,研究了杀螟松、乐果和水杨硫磷的热分解,得出一个共同的结论,即在加热贮藏中,这些有机磷农药都是先发生异构化反应,由硫酮(逐)式变成硫赶(醇)式异构体;而硫赶式异构体更不稳定,进一步分解成为聚磷酸,同     

工业和精制六六六

1.规格 1.1 原药本品主要含有1,2,3,4,5,6-六氯环己烷异构体的混合物,为白色至浅褐色颗粒、薄片或粉末,不含有外来杂质或添加的改性剂。 1.2 化学和物理的技术条件从出售商品的任一部分取样(方法见WHO/M/1)都应符合1.1节及下列的技术要求:     

气相色谱法测定杀螟丹的残留量

一、原理该法基于将杀螟丹原药溶解在酸性水溶液中,然后再转入含有氯化镍的氨水中,经水解生成1,3-双巯基2-(N,N-二甲胺基)丙烷的镍螯合物。此螯合物能定量地氧化成更稳定的沙蚕毒:4-(N,N-二甲胺基)-1,2-二硫噻烷。样品的制备包括用有机溶剂提取沙蚕毒和用液-液分配法将其净化。气相色谱法的特点是采用火焰光度检测器中的硫滤光片(394nm),因此对样品中杀螟丹的测定有特定的选择性,而免去其它杂质的干     

京博高手性比茚虫威原药投产

<正>近日获悉,京博农化已经顺利投产异构体比例9:1茚虫威原药(S体含量为90%),并实现规模化生产,产品质量达到国际先进水平。茚虫威为杜邦研发,1998年上市之初即为市场带来防控鳞翅目昆虫的独特作用模式。经过多年的商品化应用,其高效、低毒且不易产生交互抗性得到市场的广泛认可。迄今为止,茚虫威已在全球超过75个国家登记和上市,适用作物主要为棉花,其次为果蔬。2013年茚虫     

丁草胺原药中主要杂质的GC-MS定性分析

利用气相色谱-质谱联用(GC-MS)技术对丁草胺原药中的主要杂质进行定性分析。实验选用色谱柱为DB-5Ms30m×0.25mmID,电离方式为电子喷雾(EI)和化学电离(CI)。从总离子图中可以看出丁草胺中共有11种主要组分,其中10种杂质。根据质谱数据推断出11种组分的结构式,并利用丁草胺标样的质谱数据对丁草胺有效成分进行了确认。推断结果可知,丁草胺原药中存在联合国粮农组织对丁草胺原药有限量的杂质成分二丁氧基甲烷和2-氯-N-(2,6-二乙基苯基)乙酰胺。     

Behavior of N-methylcarbamate pesticides during refinement processing of edible oils

The following N-methylcarbamate pesticides, aldicarb, aldicarb sulfoxide, aldicarb sulfone, oxamyl, methomyl, thiodicarb, propoxur, carbofuran, carbosulfan, benfuracarb, bendiocarb, carbaryl, fenobcarb and furathiocarb, were added to soybean oil, each at 5 mg/kg(5 ppm), followed by degumming, alkali refining, bleaching and deodorization for oil refinement. Residual pesticide content in each case was determined immediately after refining. DEGUMMING: Aldicarb, aldicarb sulfoxide, aldicarb sulfone, oxamyl, thiodicarb, carbosulfan, benfuracarb were each found to decrease by as much as 70% by H(3)PO(4) treatment, this being less than 26% noted for the other pesticides. With hot water treatment, the decrease in any one pesticide was less than 52%. ALKALI REFINING: The rate of decrease varied with the pesticide, ranging from 8% to 100%. 200%NaOH were effectively brought about pesticide removal, compared to 125%NaOH. BLEACHING: Aldicarb, aldicarb sulfoxide, aldicarb sulfone, oxamyl, methomyl, thiodicarb, carbosulfan, benfuracarb, bendiocarb and furathiocarb each decreased by more than 80% with activated clay containing activated charcoal. Carbaryl decreased remarkably by this clay. Pesticide removal in all cases was at less than 30%. DEODORIZATION: 40% Furathiocarb, 14% carbosulfan, 11% benfuracarb and 3% carbofuran could still be detected subsequent to deodorization at 260 degrees C while all other pesticide amounts were too small to permit quantitative detection. Degumming with H(3)PO(4) and bleaching with activated clay caused the conversion of carbosulfan and benfuracarb into carbofuran. Carbofuran and furathiocarb may thus possibly still remain in the oil following the above 4 refinement processes.     

苯氧菌酯的合成研究

以苯酞和邻甲酚为起始原料 ,生成物经酰氯化、酰氰化、水解反应得苯基草酸甲酯衍生物 ,再与甲氧基氨盐酸反应得Z/E构型混合物。该混合物经转位反应得苯氧菌酯。反应总收率为 5 7 2 % (以苯酞计 ) ,产品纯度为 95 %。该工艺流程简单 ,易于工业化生产     

来氟米特3-甲基异构体的制备及结构确证

来氟米特3-甲基异构体（2）是一个有毒副作用的杂质,需定量分析。提供了一种制备来氟米特3-甲基异构体的方法,纯度99．5％,结构经IR、NMR、MS等光谱确证,可以作为控制来氟米特质量的杂质标准品。     

灭多威在棉花及土壤中降解动态及残留量研究

按生产上常规用量，每亩喷施２０％灭多威乳油６０毫升防治二代棉铃虫，施药后７天在棉叶上及１４天在土壤中其降解率分别为９８．８１％及８８．０９％；半衰期分别的１．５６天及４．９８天。防治二、三、四代棉铃虫，按有效剂量施药６次，有效成分７２克／亩，棉籽和土壤中的最大残留量分别为０．０２３及０．０８４微克／克；再加大５０％用量，有效成分１０８克／亩，最大残留量仅为０．０３４及０．２１４微克／克。结果表明，灭多威在棉叶上及土壤中降解较迅速，常规用量下，对棉籽及土壤污染较轻。     

25%硫双威防治棉铃虫田间试验

在第二代棉铃虫幼虫发生盛期，用２５％硫双威可湿性粉剂８００、１０００倍液喷雾防治一次，药后７天的校正防治效果分别为８６．１％和８２．１％，能把棉铃虫残虫量控制在防治指标以内。硫双威对棉铃虫天敌较安全，处理区棉铃虫天敌量，明显高于其它农药处理区。     

Field evidence of synergism and inhibition in the sesiidae sex pheromone system

The E,Z, Z,Z, and Z,E geometric isomers of 3,13 octadecadien-1-ol acetate were used singly and in binary combinations to trap sesiids in Wisconsin cherry orchards. The Z,E isomer alone did not capture any sesiids. A synergistic effect, however, of Z,E onSynanthedon pictipes response to its pheromone E,Z was demonstrated for the first time. Strong inhibitory effects of the Z,Z isomer onS. pictipes response to E,Z, and of the E,Z isomer onS. scitula response to Z,Z, were found. As little as 0.5% of Z,Z in E,Z completely inhibited theS. pictipes response. This species' response was also reduced by 85% when Z,Z was evaporated at 4 points, each ca. 6 m from the pheromone trap. Consistencies and discrepancies of the data with relevant experimental results from other geographical areas are briefly discussed.Lepidoptera: Sesiidae (=Aegeriidae), the clearwing moths.Research supported by the College of Agriculture and Life Sciences, University of Wisconsin, Madison, and by the Wisconsin Red Tart Cherry Ind. Market. Order.     

灭多威及其混合剂对棉铃虫的杀卵作用和生化机理

用灭多威及其混合剂处理不同发育阶段的棉铃虫卵和初孵幼虫，生化法测定不同发育阶段卵中的乙酰胆碱酯酶，羧酸酯酶活性和蛋白质含量。结果表明，灭多威及其混合剂对初产卵杀卵作用较小，对发育至１日龄以后卵的杀卵作用大；３种混合剂对初孵幼虫的击倒毒力均高于灭多威；该类药剂杀卵作用大小与卵内乙酰胆碱酯酶的活性呈正相关。     

灭多威生产技术的改进

研究了氯化反应时间和反应温度对灭多威中间体收率的影响，优化了反应条件，并改造了灭多威反应器的内部结构，使灭多威原粉的总收率提高了１８．２％，获得了良好的经济效益     

Evidence for (E,Z)-8,10-dodecadienyl acetate as the major component of the sex pheromone of the eastern pine seedworm,Cydia toreuta (Lepidoptera: Tortricidae)

The sex pheromone ofCydia toreuta (Grote), the eastern pine seedworm, was investigated using electroantennogram (AG) measurements, gas chromatography (combined GC-FID-EAD) measurements, and field tests. (E,Z)-8,10-dodecadienyl acetate (E,Z8,10-12:Ac) and (E,E)-8,10-dodecadienyl actetate (E,E8,10-12: Ac) produced both the highest EAG and EAD responses. Only a single antennal stimulatory peak was observed when female abdominal tip extracts were analyzed by GC-FID-EAD, which corresponded exactly with that of authenticE,Z8,10-12: Ac. Field tests confirmedE,Z8,10-12: Ac as the major pheromone component. TheE,Z isomer by itself caught equivalent numbers of male moths as did caged females. The addition of theE,E isomer to theE,Z form increased trap catch, although not significantly (P = 0.05). The addition of (Z,Z)-8,10-dodecadienyl acetate to theE,Z isomer significantly (P=0.05) reduced trap catch, while the addition of (Z,E)-8,10-dodecadienyl acetate to theE,Z form also decreased trap catch, but not significantly (P=0.05).