反相高效液相色谱法测定混合制剂中辛硫磷和久效磷的含量

采用以７０％甲醇为流动相的反相高液相色谱法测定混配乳油中的辛硫磷和久效磷，以外标法定量，结果表明：辛硫磷和久效磷含量测定的平均回收率分别为１００．２６％和９９．０３％，６次重复测定的变异系数分别为０．７５％和０．８４％。产品中的杂质与有效成分分离完全，对测定无干扰。一交进样分析的时间约为６分钟。     

高效液相色谱法测定21%丁硫克百威·辛硫磷乳油中有效成分含量

[目的]建立高效液相色谱法同时测定丁硫克百威和辛硫磷的含量。[方法]试样用甲醇溶解,采用梯度洗脱的方法,以甲醇-水为流动相,同时对丁硫克百威和辛硫磷进行分离,外标法定量。[结果]测定辛硫磷的方法线性相关系数为1.0000,变异系数为0.41%,平均回收率为99.9%;测定丁硫克百威的方法线性相关系数为0.9999,变异系数为0.90%,平均回收率为97.2%。[结论]方法满足农药产品含量分析的要求,可同时测定丁硫克百威和辛硫磷的含量。     

棉铃宝高效液相色谱分析方法研究

本法采用同一色谱条件反相高效液相色谱法测定棉铃宝中甲基对硫磷和辛硫磷的含量，方法简单易行，具有较高的精密度和准确度，其回收率分析为甲基对硫磷９９．５９％，辛硫磷１０１．０％。     

毛细管气相色谱法测定地表水中甲拌磷和乙拌磷

本文建立了二氯甲烷液液萃取地表水样品,气相色谱法同时测定水中甲拌磷和乙拌磷的方法。本方法前处理操作简单,富集效率高,分析方法检出限低,精密度和加标回收率符合分析测试要求,适用于地表水中甲拌磷和乙拌磷的测定。     

高效液相色谱法测定混合制剂中甲基对硫磷和辛硫磷含量

高效液相色谱法测定混合制剂中甲基对硫磷和辛硫磷含量许良忠，张书圣，于永良（青岛化工学院应化系）甲基对硫磷和辛硫磷是目前防治棉铃虫的优良药剂，二者混配对棉铃虫有一定增效作用，所组成的混剂对抗性棉铃虫防效突出。甲基对硫磷和辛硫磷的国标分析方法分别是采用气...     

分子印迹固相分散萃取-液相色谱法测定甘薯中毒死蜱与辛硫磷残留量

[目的]建立以分子印迹固相分散萃取结合液相色谱法测定甘薯中毒死蜱与辛硫磷残留量的方法,为甘薯食品安全研究提供依据。[方法]以表面印迹聚合方法合成毒死蜱分子印迹聚合物,该聚合物对毒死蜱有特异性吸附,对辛硫磷也具有一定的吸附性能,采用该印迹聚合材料作为固相分散萃取剂进行甘薯中毒死蜱及辛硫磷的残留测定。[结果]结果满足分析要求,方法在0.005~3.0 mg/kg的范围内线性关系良好,方法的检出限分别为0.571(毒死蜱)、0.826μg/kg(辛硫磷);回收率为68.4%~101.6%。[结论]该方法简单快速,可用于甘薯中毒死蜱及辛硫磷的残留测定。     

高效液相色谱法测定兽药克螨威中辛硫磷的含量

克螨威为驱杀家畜体外寄生虫的外浴兽药 ,主要含有辛硫磷其含量测定方法有气相色谱法〔1〕等。本文采用高效液相色谱法测定其含量〔2〕以十八烷基硅烷键合硅胶为填充剂 ,以乙腈—水 (54∶ 46 )为流动相 ,检测波长 2 6 0 nm,以峰面积测定辛硫磷的含量。该方法具有简便、快速、准确等优点。适用于该产品质量检验分析     

药剂拌种防治农田害鼠

甲拌磷、甲基异柳磷拌种对小麦地下害虫有较好的防治效果,而对农田害鼠的兼治作用尚未见报道。我们于1984-1985年对国内生产的主要应用于拌种的药剂甲拌磷、甲基异柳磷、辛硫磷进行了室内和田间试验,现简报如下。一、试验方法(一)室内毒力测定采用饲喂法,即按种子量0.2%将50%甲拌磷(济宁农药厂)、40%甲基异柳磷(胶县农药厂)、50%辛硫磷(临沂农药厂)拌成小麦毒饵,对黑线姬鼠进     

辛硫磷高效液体色谱分析

色谱柱分离辛硫磷及其杂质能够达到理想的效果,但是辛硫磷具有热不稳定性,所以至今国内未见用气相色谱法分析辛硫磷的报道,采用高效液体色谱分析辛硫磷能克服辛硫磷对热的不稳定。我们用反相液—液色谱制取了辛硫磷及其杂质的分离谱图,并以邻苯二甲酸二丁酯为内标物进行了定量分析。     

农药杀虫剂辛硫磷纯品的制备及鉴定

一前言工业生产中辛硫磷的纯化通常采用减压蒸馏的方法,此法只能除去低分子量的杂质,而且由于它的光热稳定性不好,难以避免新的分解产物生成,因此很难得到纯度高的样品。为了开展辛硫磷残留分析工作的需要,我们研究了从辛硫磷工业原油分离制备纯品的方法。实验中采用柱色谱法——薄层色谱法对工业辛硫磷原油进行了分离纯化研究,并得到了满意的结果。     

甲拌膦高效液相色谱检测方法研究

目的探讨高效液相色谱法检测甲拌膦的方法。方法采用不同的流动相、检测波长等反复测定甲拌膦的峰面积与峰高,按照规定的标准方法对本试验条件检测甲拌膦的检测限、线性范围与产品及加标回收率的实验。结果在流动相乙腈+水(85+15)、205 nm波长,甲拌膦在5.1 min附近产生一灵敏色谱峰,线性范围为:0.02~2.5μg,检出限为:0.005μg。结论高效液相色谱在一定条件下测定甲拌膦的含量效果理想。     

SO2-4／TiO2-ZrO2固体酸催化剂催化废弃动植物油脂制备生物柴油

制备了SO2-4/TiO2-ZrO2固体酸催化剂,并以其催化废弃动植物油脂与甲醇发生酯交换反应制备生物柴油.结果表明,催化剂SO2-4-/TiO2-ZrO2表现出了较高的催化活性,在反应压力343 kPa下的最佳酯交换反应条件为:反应温度125℃、醇油摩尔比10∶1、催化剂用量5％、反应时间3h,该条件下废弃动植物油脂...     

昆虫病原线虫对花生田蛴螬的防治效果

利用蛴螬的病原线虫于花生下针期穴施1．5～2万条，收获前进行田间调查。研究结果表明，病原线虫1号、2号[Rhabditis（Oscheius）spp）制剂防治花生田蛴螬效果分别达96．6％和96．1％，花生增产91．3％和91．6％，均好于辛硫磷。     

Phorate degradation by TiO2 photocatalysis: Parameter and reaction pathway investigations

The photocatalytic degradation of phorate in aqueous suspensions was examined with the use of titanium dioxide (TiO₂) as a photocatalyst. About 99% of phorate was degraded after UV irradiation for 60 min. The photodegradation of phorate followed pseudo-first-order kinetics and parameters such as pH of the system, TiO₂ dosage, and presence of anions were found to influence the reaction rate. To obtain a better understanding of the mechanistic details of this TiO₂-assisted photodegradation of phorate with UV irradiation, the intermediates of the processes were separated, identified, and characterized by the solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) techniques. The probable photodegradation pathways were proposed and discussed. To the best of our knowledge, this is the first study that reports the degradation pathways of phorate. The electrical energy consumption per order of magnitude for photocatalytic degradation of phorate was also calculated and showed that a moderated efficiency (E_EO = 96 kWh/(m³ order)) was obtained in TiO₂/UV process.     

甲拌磷降解菌XT2的分离鉴定及其降解特性

[目的]选用新疆石河子市周边受甲拌磷污染的土壤为菌源进行研究,从而获得有效降解有机磷农药甲拌磷的微生物.[方法]以甲拌磷作为唯一碳源和能源采用逐渐加量的驯化方式.[结果]分离得到1株对甲拌磷有一定降解能力的降解菌XT2,根据其形态特征、生理生化特性及16S rDNA序列分析,将其鉴定为斯氏普罗威登斯菌(Providencia stuartii),该菌能以甲拌磷作为唯一碳源生长,接种该菌于500 mg/L的甲拌磷基础盐液体培养基中,120 h时甲拌磷降解率可达77.89%.[结论]筛选获得了1株能有效降解甲拌磷的细菌,被鉴定为斯氏普罗威登斯菌.     

Removal of Organophosphorus Pesticides from Aqueous Solution by Using Adsorptive Bubble Separation Techniques

Abstract

Two organophosphorus pesticides, ddvp (phosphoric acid 2,2-dichlorovinyl dimethyl ester) and phorate (phosphorodithioic acid o,o-diethyl s-[(ethylthio)methyl] ester) were removed from aqueous solution by three adsorptive bubble separation techniques: air stripping, solvent sublation, and adsorbing colloid flotation. The effects of pH, flow rate, surfactant, ethanol, ionic strength, and coprecipitant concentration on the efficiency of pesticide removal were studied. Over 97% of phorate was removed in 30 min by solvent sublation, and 90% of phorate was removed in 10 min by adsorbing colloid flotation with Fe(OH)₃, floc. The separations of ddvp by these techniques were not effective.     

Rapid analysis of fatty acids in plasma lipids

A rapid and convenient procedure for the quantitative determination of the fatty acid composition of plasma lipids is described. Human plasma was applied directly to the preadsorbent zones of thin-layer silica gel plates with added antioxidant, internal standards and carriers. The thin-layer chromatography (TLC) plates were partially developed with methanol followed by chloroform/methanol (1∶1, v/v), and then they were fully developed in hexane/diethyl ether/acetic acid (80∶20∶1, v/v/v) to separate the major classes of lipids. Silica gel from regions containing the separated lipids was scraped into screw-capped tubes and treated with boron trifluoride-methanol prior to gas chromatography. The method of direct application to TLC plates gave yields and compositions of fatty acids very similar to the method of applying extracted plasma lipids. This relatively simple method is suitable for analyzing the fatty acids in plasma lipids from a 50 microliter finger-tip blood samples from an individual, and it may be useful in wide-scale screening of different individuals to estimate the relative amounts of ingested polyunsaturated fatty acids. Pfizer Biomedical Research Awardee.     

溴乐菊酯乳油中溴氰菊酯和乐果含量的测定

本文采用具有分离手段的薄层层析，选择合适的展开剂，经分离后，分别刮下溴乐乳油中溴氰菊酯和乐果斑条，采用紫外分光光度法在波长276的纳米处理进行溴氰菊酯含量测定，采用化学溴化法进行乐果含量测定，该法简便，准确可靠，重复性好，可作为产品质量控制和检测方法。     

刮壁搅拌桨的最优设计

运用罚函数Ｇａｌｅｒｋｉｎ加权余量有限元数值算法模拟了Ｖｏｔａｔｏｒ、Ｃ＆Ｒ反应器和刮壁槽式釜中轴截面的流速和剪切分布。计算结果表明，Ｖｏｔａｔｏｒ，Ｃ＆Ｒ反应器中流动和剪切分布较刮壁槽式釜更有利于流体的混合和壁面的传热。对Ｃ＆Ｒ反应器，采用无间隙刮板，其传热和混合性能优于有间隙刮板。建议刮壁搅拌反应器的设计采用类似Ｖｏｔａｔｏｒ和Ｃ＆Ｒ反应器的环隙结构和无间隙的刮板形式。     

甲拌磷农药废水的光催化降解

对光稳定、生物难降解的甲拌磷农药废水经ＴｉＯ２或负栽型ＴｉＯ２光催化降解方法处理,化学耗氧量达到排放标准。研究了ＰＨ值、阴离子种类对降解过程的影响,ＰＨ〈２或ＰＨ〉８时,降解率高于５０％。催化剂稳定性好;当ＣＯ３＾２－和ＳＯ３＾２－离子质量浓度约为６．０ｍｇ／Ｌ时降解率下降２０％。