香蕉中噻唑膦残留分析方法研究

建立香蕉中噻唑膦的超高效液相色谱串联质谱法(UPLC-MS/MS)残留测定方法。香蕉样品采用乙腈提取和PSA+C18分散固相萃取,采用UPLC-MS/MS多反应模式(MRM)进行分析测定。噻唑膦在添加水平0.01~1.0 mg/kg范围内,平均回收率为94.3%~107.5%,相对标准偏差为7.9%~11.0%。采用外标法定量,方法的检出限为0.001μg/m L,定量限为0.005 mg/kg。该方法简单、准确、重复性较好且节省溶剂,适用于香蕉中噻唑膦的残留检测。     

Residue management for reducing evaporation in relation to soil type and evaporativity1

Abstract. Usual residue-management options are to remove the residue, use it as mulch with or without undercutting or to incorporate it into the soil. While the role of surface mulch in evaporation has been widely studied, the information on the effect on evaporation of mulch with undercutting or residue incorporated into soil, particularly in relation to soil type and evaporativity (E_o) is lacking. We studied the effect of wheat straw used in various ways on the course of evaporation loss from soil columns with three soils at Ludhiana, India and one soil at Bushland, Texas, USA, under two E_o's Energy-limited evaporation rates under mulch (E_om) followed the soil-specific relation E_om/E_o= a e^(bRes+cEo), where Res is residue rate t/ha and a, b and c are constants; E_o, is expressed in mm/d. In an effort to model the total evaporation (CE) during the energy-limited stage ‘U’ was obtained from appropriate CE versus time curves and (CE-U) was regressed over (t - ti)^0.5 to obtain the slope ‘α’ (Ritchie 1972) for the soil-limited evaporation stage. The observed ‘U’ was independent of mulch rate and E_o but was strongly affected by soil type, Values of ‘α’ decreased with increase in mulch rate and decrease in E_o and coarseness of soil. The otherwise short lived benefit of evaporation reduction with mulch per se, which peaked after a few days was maintained when residue was mixed with soil at the stage when evaporation reduction reached a maximum; this benefit continued for several weeks. Cumulative evaporation values computed from ‘U’ and ‘α’ agreed closely with the observed values under straw mulch for loamy sand and clay loam soils and for ‘undercut’ and ‘residue mixed’ treatments on all soils regardless of E_o, and for all situations under small E_o. However, for sandy loam and silt loam soils under E_o of 10 mm/d, the modified square root of the time function of Jalota et al. (1988) gave a better fit.     

我国农药残留快速检测技术的研究与应用现状

本文简述了目前农药残留快速检测技术的研究概况，分析了农药残留快速检测技术在我国的实际应用情况。     

动物组织中己烯雌酚残留的高效液相色谱/电化学检测方法研究

建立了动物组织中己烯雌酚的高效液相色谱/电化学检测方法.色谱柱为HypersilODSC18柱(5μm,4.6mm×250mm);流动相为乙腈-0.007mol/L磷酸二氢铵(48∶52,V/V,pH3.5);电化学检测的检测模式为前处理(pretreat),工作电压为0.9V,灵敏度为0.5μA.己烯雌酚浓度在0.2～100ng/g范围内具有良好线性关系,相关系数为0.9995.各组织不同添加浓度的平均回收率均为80%,批内变异系数《3.60%,批间变异系数《3.72%,检测限为0.2ng/g.     

司帕沙星在雏鸡体内药代动力学及残留的研究

选用30日龄健康海兰鸡65只,按5mg／kg体重口服给予司帕沙星,定期采样,以高效液相色谱法测定血浆、肝、肾、心、肺和肌肉中司帕沙星的含量,研究司帕沙星在鸡体内的药动学与残留。结果表明:司帕沙星在血液中经时过程符合一级吸收二室开放模型,其主要动力学参数如下:t1／2α0.9585h,t1／2β11.7447h,tmax0,6514 h,Cmax0.5271 μg／ml,AUC1.7908mg／L／h。肾脏、心脏的药时数据符合一级吸收二项指数方程,其主要动力学参数分别为:t1/2Ka0.3733 h、0.1530h,t1／2k1.3007 h、2.1013h,tmax1.01420h、0.6239 h,Cmax2.1104μg／ml、1.6721 μg／ml,AUC6.51764 mg／L／h、6.2286mg／L／h。司帕沙星在肝脏、肺脏、肌肉中的经时过程符合一级吸收三项指数方程,主要动力学参数分别为t1/2α0.3672 h、0.6156 h、1.5835 h,t1/2β3.9998 h、15.0271 h、12.0103h,tmax0.7458 h、0.7322 h、1.3726 h,Cmax4.4709μg／ml、2.5267μg／ml、0.9760μg／ml,AUC20.893 mg／L／h,27.242 mg／L／h、9.7943mg/L/h。建议司帕沙星在鸡体内的休药期为7d。     

Effect of recent cropping history and herbicide use on the degradation rates of isoproturon in soils

Five soil samples were taken from each of five fields with different crop management histories. Three of the fields were in an arable rotation, the fourth field was temporary grassland, and the final field was under permanent grass. Of the three arable fields, two had been cropped with winter wheat in three of the preceding 6 years, and the third had last been cropped with winter wheat once only, 6 years previously. With one exception, the winter wheat had been sprayed with the herbicide isoproturon. The rate of isoproturon degradation in laboratory incubations was strongly related to the previous management practices. In the five soils from the field that had been treated most regularly with isoproturon in recent years, <2.5% of the initial dose remained after 14 days, indicating considerable enhancement of degradation. In the soils from the field with two applications of the herbicide in the past 6 years, residues after 27 days varied from 5% to 37% of the amount applied. In soils from the other three sites, residue levels were less variable, and were inversely related to microbial biomass. In studies with selected soils from the field that had received three applications of isoproturon in the previous 6 years, kinetics of degradation were not first‐order but were indicative of microbial adaptation, and the average time to 50% loss of the herbicide (DT₅₀) was 7.5 days. In selected soils from the field that had received just one application of isoproturon, degradation followed first‐order kinetics, indicative of cometabolism. Pre‐incubation of isoproturon in soil from the five fields led to significant enhancement of degradation only in the samples from the two fields that had a recent history of isoproturon application.     

那西肽对生长肥育猪的作用效果及其在产品中的残留

选择32头30kg左右健康的二元杂交生长猪, 随机分为4组, 每组8头, 个体饲喂, 4组均喂相同的基础饲粮, 但添加不同饲用抗生素,分别是低、高剂量那西肽(10mg/kg、50mg/kg)、盐霉素(30mg/kg) 和对照。猪体重达90kg时, 分别按0、3和7d停药后屠宰, 检测那西肽在样品各器官中的残留量。结果表明: 那西肽可显著提高生长肥育猪的采食量和日增重(P<0 05), 但是对料重比的改善作用不明显; 当检测灵敏度为0 01mg/kg时, 在低、高剂量那西肽组猪的心脏、肝脏、肾脏和背最长肌中, 均未检出那西肽。     

猪肾脏中氯丙嗪和异丙嗪残留检测方法的建立

建立了猪肾脏中氯丙嗪和异丙嗪残留量检测的高效液相色谱法。猪肾脏中残留的氯丙嗪和异丙嗪,用乙腈提取,再依次用酸化乙腈和正己烷净化,氮气吹干,甲醇溶解后,用Waters高效液相色谱系统,HypersilC18柱,UV检测器,用V(乙腈)∶V(水)∶V(0.5mol·L-1乙酸铵)(50∶49∶1)为流动相,流速1.2mL/min,波长254nm测定,内标法定量。结果表明,氯丙嗪和异丙嗪在猪肾脏中的最低检测限均为10μg/kg,组织中添加量为10μg/kg时,氯丙嗪和异丙嗪的回收率分别为83%和84%,批间变异系数均小于20%。该方法样品处理简单,可同时检测氯丙嗪和异丙嗪在猪肾脏中的残留量。     

论蔬菜农药残留中“人”的作用

着重从生产者的角度出发,综述了我国农药使用及蔬菜农药残留状况,总结了农药残留的规律;探讨了生产者在农药残留中的重要作用和现象发生的原因;从人的根本上提出了解决问题的方法。     

金银花中戊唑醇、苯醚甲环唑的残留分析

为解决金银花种植过程中农药的使用问题,以金银花为试验对象,选用广谱杀菌剂戊唑醇和苯醚甲环唑,采用常量、倍量、二次和三次灌根处理,对最终的残留含量进行分析。头茬花各处理中苯醚甲环唑均未检出,而二茬花中戊唑醇的残留量为0.14~0.22 mg/kg,存在残留超标风险。建议使用10%苯醚甲环唑4000倍液灌根处理,防治金银花土传病害,灌根2~3次,安全间隔期15天。