超快速高效液相色谱法测定普通白菜中16种氨基甲酸酯类农药残留

研究应用超快速高效液相色谱仪柱后衍生荧光检测器同时测定普通白菜中16种氨基甲酸酯类农药残留。对流动相组成、波长选择、梯度洗脱等条件进行比较研究,建立了样品经乙腈提取,SPE-NH2固相萃取柱净化,液相色谱柱后衍生分离,荧光检测(λex＝339 nm, λem＝445 nm)测定,外标法定量的检测方法。研究表明：基于液相色谱荧光检测条件,16种农药残留在0.025～1.0 mg/L浓度范围内线性关系良好;检出限0.002～0.010 mg/L;平均加标回收率73.0%～103.0%,相对标准偏差(RSD)1.5%～8.8%。该研究确定的方法具有检测范围广、快速、灵敏、准确、重现性好、易推广等特点。     

Acute aldicarb toxicity in dogs: 15 cases (2001–2009)

Objective – To describe the common clinical signs, laboratory abnormalities, treatment, and prognosis associated with acute aldicarb toxicosis in dogs. Design – Retrospective observational study from 2001 to 2009. Setting – Urban referral hospital. Animals – Fifteen client‐owned dogs. Interventions – None. Measurements and Main Results – The most common clinical signs associated with acute aldicarb toxicosis were vomiting, ptyalism, diarrhea, and tremors. Of the 15 dogs, 11 were admitted to the hospital for treatment, 2 were euthanized at presentation and 2 were discharged against medical advice following minimal treatment and lost to follow‐up. Laboratory abnormalities included lactic acidosis and hyperglycemia in 12 and 9 patients, respectively. Treatment of hospitalized dogs included induction of emesis with apomorphine (4 dogs), activated charcoal (5), IV fluids (11), atropine (7), methocarbamol (3), diazepam (1), pralidoxime (1) and diphenhydramine (1). Ten of 11 hospitalized dogs survived to discharge; 1 was euthanized following a respiratory arrest after 36 hours of hospitalization. One patient received mechanical ventilation and treatment for pneumonia before discharge from the hospital. The median duration of hospitalization was 22 hours (range 12–168 h). Conclusions – Acute aldicarb toxicosis carries a good prognosis for survival and hospital discharge with treatment. Supportive care should be considered for at least 18–24 hours to monitor for response to therapy and development of respiratory failure.     

Studies on the Purification and Characterization of Soybean Esterase, and Its Sensitivity to Organophosphate and Carbamate Pesticides

Soybean esterase, a cholinesterase-like enzyme, was purified by differential centrifugation firstly, then, ammonium sulfate precipitation, dialysis, and finally, DEAE-cellulose-32 ion-exchange chromatography after extracting it from soybean seeds with phosphate buffer （0.3 mol L^-1, pH 7.0）. The extract recovery rate of the purified enzyme was 8.18% and purification fold was 91.58. The soybean esterase appeared as two bands on the denaturing SDS-PAGE with molecular weights of 24 and 37.2 kDa, respectively, which proved that it is a dimer protein consisting of two subunits. The result of nondenaturing PAGE revealed that the soybean esterase is a single band with cholinesterase-like activity using α- naphthyl acetate as the substrate and fast blue B salt as coloring agent. The esterase showed very high sensitivity to 18 kinds of organophosphate pesticides and 6 kinds of carbamate pesticides with the lowest detective limits of 0.03125- 0.0625 and 0.03125-0.25 mg kg^-1, respectively, and can meet the demands of MRL specified by the most countries.     

杀螺药物研究──碳酸酯、氨基甲酸酯类化合物的合成及其构效关系初步探讨

合成了碳酸酯类化合物23个和苯氨基甲酸苯酯类化合物7个。杀螺初筛试验发现，8个碳酸酯化合物具有杀螺活性，其中，化合物I1和I11，10ppm的杀螺率为100％和96．7％。碳酸苯酯的苯环上，用硝基或3个以上的氯原子取代，有利于增强该类化合物的杀螺作用。杀螺效果较好的三氯苯碳酸酯改变成同电异素体类似物，苯氨基甲酸酯后，杀螺作用明显下降。     

Carbamate poisoning in a dairy goat herd: Clinicopathological findings and therapeutic approach

Abstract

CASE HISTORY: Approximately 1 hour after the consumption of carnations from a nearby glasshouse 55 animals from a dairy goat herd exhibited signs of possible poisoning.

CLINICAL FINDINGS: Upon clinical examination affected animals exhibited signs of salivation, tympany, tachypnoea, polydipsia, urination, diarrhoea, bradycardia, miosis, tremor and convulsions. As poisoning from an acetylcholinesterase-inhibiting insecticide was suspected, treatment with atropine sulphate was initiated at a dose of 0.3 mg/kg bodyweight. The treatment was repeated for some animals that relapsed, and was effective in all cases, with the exception of one goat kid that died.

DIAGNOSIS: Necropsy of the goat kid showed pulmonary oedema and congestion of internal organs. Toxicological analysis of stomach contents and liver of the dead animal, as well as of the carnations, revealed high concentrations of carbamates.

CLINICAL RELEVANCE: Carbamate poisoning after consumption of polluted feedstuffs or glasshouse products can be fatal for dairy goats. Atropine sulphate, at 0.3 mg/kg, can be useful in treating this condition.     

N-(6-氯吡啶-3-基)羰基-2-取代芳基磺酰胺的合成、结构及除草活性研究

以邻苯二甲酸酐、磺胺和氯甲酸丁酯为原料,通过活性亚结构拼接合成了一个系列20个新型酰基磺酰亚胺类衍生物3a~3t,其结构均经过了¹H NMR、¹³C NMR 和高分辨质谱确证。分别采用菌丝生长速率法和茎叶喷雾法测定了目标化合物的抑菌活性和除草活性。抑菌活性测定结果显示：在50 mg/L下,大部分化合物对油菜菌核病菌、茶叶炭疽病菌、白芨白绢病菌和辣椒疫霉具有较好的抑制作用;化合物3f、3n和3q对油菜菌核病菌的抑制率分别为63.98%、79.56%和77.83%,优于对照药剂磺草灵(58.78%);化合物 3q对油菜菌核病菌、茶叶炭疽病菌的EC₅₀值分别为10.49 mg/L和21.57 mg/L,优于磺草灵。除草活性测定结果显示,在150 mg/L 时,化合物3a对稗草的鲜重防效为52.48%,低于磺草灵(71.68%)。本研究所合成的新型酰基磺酰亚胺类新化合物具有较好的抑菌活性,可为新型酰基磺酰亚胺衍生物的抑菌活性研究提供参考。

     

环境样品氨基甲酸酯类农药的分离和检测技术研究进展

氨基甲酸酯类农药是一类高效广谱型杀虫剂,近年来在农业生产中被广泛使用,然而由此带来的环境污染和食品健康问题也日益引起关注。无论是样品的前处理方法还是仪器检测方法都有待不断地完善和发展,因此,开发理想的样品前处理方法和更加有效的仪器分析方法成为该领域的研究热点。本文在查阅了近年国内外相关文献60篇的基础上,就环境样品氨基甲酸酯类农药的分离提取方法以及不同方法的优缺点作分析,同时对氨基甲酸酯类农药的仪器分析方法及其发展趋势作总结,以期为环境样品氨基甲酸酯类农药的分析技术研究提供有益的参考。     

Effects of tea tree oils on removing pesticide residue in cowpea

为研究茶树油清除果蔬农药残留的效果,该试验选取豇豆为供试材料,以不同浓度的茶树油和水溶性茶树油等清洗处理,利用气相色谱和气相色谱-质谱联用检测豇豆内有机磷类、拟除虫菊酯类和氨基甲酸酯类的农药残留量,计算农药清除率。供试7种农药中,水胺硫磷、马拉硫磷、氧乐果、三唑磷、毒死蜱、氯氰菊酯和速灭威在豇豆中的初始浓度分别为：20.395、1.690、6.524、10.719、0.160、12.104和23.057 mg/kg。茶树油处理后检测结果表明,茶树油具有清除残留在豇豆中农药的能力,清除效果随茶树油浓度增加而增强;清除有机磷类农药效果较拟除虫菊酯类和氨基甲酸酯类农药明显。茶树油比去离子水、市售果蔬农残清洗剂清除农药残留效果显著,同时,相同浓度的水溶性茶树油比相应茶树油清除农药残留能力强。0.8%水溶性茶树油清除效果最佳,清除率分别为水胺硫磷80.48%,马拉硫磷94.54%,三唑磷82.79%,毒死蜱84.58%,氧乐果72.20%,氯氰菊酯80.51%,速灭威72.21%。通过研究结果可知,茶树油可作为有开发前景的果蔬清除剂。     

高效液相色谱柱后衍生化法检测玉米粉中的氨基甲酸酯类农药残留

本文建立玉米粉中几种氨基甲酸酯类农药残留量的测定方法,样品用乙酸乙酯提取,以LC-FlorisilSPE小柱净化,采用高效液相柱后衍生化法系统、荧光检测器检测。方法对5种氨基甲酸酯类农药的最低检出浓度在0.0032～0.0044mg/kg,回收率在82.5%～97.3%之间,变异系数在均<6.2%。