QuEChERS-超高效液相色谱-质谱联用法测定熊胆粉中9种苯二氮䓬类药物残留量

建立了超高效液相色谱-质谱联用法(UPLC-MS/MS)快速测定中药材熊胆粉中9种苯二氮?类药物残留的方法。样品以乙腈为提取溶剂,经萃取盐包除杂提取,采用分散式固相萃取管 (EMR-Lipid dSPE) 净化,ACQUITY BEH C18色谱柱(1.7 μm,2.1×100 mm)分离,多反应监测模式(MRM)采集数据,外标法定量。在优化的条件下,虽9种药物存在不同程度的基质效应,但不影响检测结果的准确性。方法学考察结果显示,9种苯二氮?类药物在对应的浓度范围内线性关系良好,决定系数(R²)≥0.9961,方法检出限(LOD,S/N =3)在0.06～0.71 μg/kg范围内,定量限(LOQ,S/N =10)在0.20～2.60 μg/kg范围内,3个加标水平的平均回收率在69.1%～108.0%范围内,日内RSD为1.8%～9.0%,日间RSD为2.6%～9.3%。该方法前处理操作简便、重现性好,准确度高,为熊胆粉中苯二氮?类药物残留的风险监控提供了一种有效的检测技术。     

农产品农药残留的标准、检测和降解技术的研究进展

概述了农产品中的农药残留标准现状、农药残留分析方法及存在问题和国内外降解农药残留研 究的主要成果,介绍了当前国内外在农药残留分析中应用的固相萃取、微波辅助萃取及固相微萃取等样 品前处理技术,以及在农药残留的降解脱除中应用的超声波清洗和电离辐射等物理方法、臭氧氧化技术 和光降解等化学方法、细茵和真菌等微生物降解方法等,并针对我国的实际情况提出了今后农药残留研 究的重点和方向。     

氰戊菊酯在水中的降解

氰戊菊脂在水中的降解速度与酸碱度和光照强度有关,在碱性溶液中降解快,酸性及中性溶液中降解较慢,在蒸馏水中的光解速度,直射太阳光比散射光快。氰戊菊酯在室外池塘水中很快降解,水生生物的吸附作用是影响降解速度的重要因素,在夏季有水生植物和鱼的池塘水体中的降解半衰期为0.7～1天,在无水生植物和鱼的池水中降解较慢。     

Residues of zeta‐cypermethrin in bovine tissues and milk following pour‐on and spray application

The depletion of zeta‐cypermethrin residues in bovine tissues and milk was studied. Beef cattle were treated three times at 3‐week intervals with 1 ml 10 kg^?1 body weight of a 25 g litre^?1 or 50 g litre^?1 pour‐on formulation (2.5 and 5.0 mg zeta‐cypermethrin kg^?1 body weight) or 100 mg kg^?1 spray to simulate a likely worst‐case treatment regime. Friesian and Jersey dairy cows were treated once with 2.5 mg zeta‐cypermethrin kg^?1 in a pour‐on formulation. Muscle, liver and kidney residue concentrations were generally less than the limit of detection (LOD = 0.01 mg kg^?1). Residues in renal‐fat and back‐fat samples from animals treated with 2.5 mg kg^?1 all exceeded the limit of quantitation (LOQ = 0.05 mg kg^?1), peaking at 10 days after treatment. Only two of five kidney fat samples were above the LOQ after 34 days, but none of the back‐fat samples exceeded the LOQ at 28 days after treatment. Following spray treatments, fat residues were detectable in some animals but were below the LOQ at all sampling intervals. Zeta‐cypermethrin was quantifiable (LOQ = 0.01 mg kg^?1) in only one whole‐milk sample from the Friesian cows (0.015 mg kg^?1, 2 days after treatment). In whole milk from Jersey cows, the mean concentration of zeta‐cypermethrin peaked 1 day after treatment, at 0.015 mg kg^?1, and the highest individual sample concentration was 0.025 mg kg^?1 at 3 days after treatment. Residues in milk were not quantifiable beginning 4 days after treatment. The mean concentrations of zeta‐cypermethrin in milk fat from Friesian and Jersey cows peaked two days after treatment at 0.197 mg kg^?1 and 0.377 mg kg^?1, respectively, and the highest individual sample concentrations were 2 days after treatment at 0.47 mg kg^?1 and 0.98 mg kg^?1, respectively. © 2001 Society of Chemical Industry     

果蔬农药残留快速检测固定化酶片的制作研究

[目的]对胆碱酯酶的保藏性进行研究分析,以期得到保障农药残留检测的最佳酶活力。[方法]试验选定高酶活力的大豆酯酶为酶原,通过筛选最适反应温度、反应时间、离子浓度和最适pH,及最佳的反应显色体系来确定反应最适的条件,采用不同的显色体系酶抑制法,研究酶片的制作方法。[结果]酶片载体材料采用硝酸纤维膜,制作每张酶片取20μL大豆酶液,15μL 0.5%的BSA溶液,2μL 0.05%戊二醛于平底试管中。添加0.03 mol/L pH 7.0的磷酸缓冲液至总体积100μL,4℃固定10 h;制作每张显色片,需在1 cm×1 cm大小的滤纸片上加入50μL显色剂,30μL底物,4℃冷风吹干,封膜真空保存。[结论]固兰B盐和α-乙酸奈酯组合,适合作为酶抑制法检测有机磷农药残留的显色剂,且效果明显。     

农药残留酶联免疫吸附分析技术研究进展

酶联免疫吸附分析法具有灵敏度高、特异性强、方便快捷的特点,在现场筛选和大量样品的快速检测中显示了其独特的优势。简要介绍了农药残留酶联免疫吸附分析技术的关键环节及其应用,并对该技术存在的问题和应用前景进行了讨论。     

蔬菜农药残留问题的研究进展

从蔬菜农药残留的概念、原因、为害、检测技术等方面论述了其研究进展,并针对目前生产上蔬菜农药残留量超标的现象,提出相应的解决方法。     

Analysis of sawn lumber production from logging residues of branchwood of <Emphasis Type="Italic">Aningeria robusta</Emphasis> and <Emphasis Type="Italic">Terminalia ivorensis</Emphasis>

One way of meeting the supply demands of the wood industry is through the reduction of waste in timber processing. It has been estimated in Ghana that for every tree felled, nearly 50% of the tree volume is left in the forest in the form of branches, crownwood, and stumps. In this study, the potential of utilizing branchwood as raw material from logging residues to help meet the timber demands of the downstream processing sector was analyzed experimentally. The sawing characteristics of the branchwood of Aningeria robusta and Terminalia ivorensis with diameters in the range 10–25 cm using live sawing and cant sawing methods were determined using a randomized complete block design, 2 × 4 factorial with three replications. Experimental results indicate that, the relative lumber value yields for first and second grade boards of A. robusta and T. ivorensis branches were 25 and 20%, respectively, while the green lumber volume yields were 40 and 32%, respectively. A high proportion of sapwood and the occurrence of washboarding in T. ivorensis contributed to that species’ relatively low lumber value and volume yield. The experimental results further indicate that the sawing technique used had no significant influence on lumber yields. However, at 5% level of significance, significant differences in lumber yield existed between some of the diameter classes.     

常绿阔叶林迹地炼山营造杉木林群落演替趋向调查初报

据样地调查，该２５年生杉木人工林群落的植物有４１科８４属１２０种，群落的外貌特征以包括藤本在内的高位芽占绝对优势，叶特征以革质，单叶，中小型叶为主，由于该群落的幼树层以米储和木荷等占优势，若让其自然发展或杉木林采伐后不炼山，并排除其它人为干扰，该群落将向与常绿阔叶林采伐前的群落类型相似的方向演替。     

3种内吸农药分子印迹聚合物制备及初步应用

【目的】制备3种内吸性农药分子印迹聚合物及固相萃取柱,建立MISPE-LC-MS/MS方法。【方法】应用分子印迹技术制备分子印迹聚合物,通过研究模板分子、功能单体和交联剂的配比关系以及索氏萃取效率,分析该聚合物制备的影响因素;通过吸附试验分析该聚合物特异性;通过研究不同洗脱溶剂、洗脱体积等因素对该萃取柱的使用进行优化,最后通过对黄瓜样品添加回收率测定分析该方法的实用性。【结果】制备出了多目标物特异性分子印迹聚合物,其对嘧菌酯、噻虫啉和吡虫啉具有较高识别能力和快速吸附效果,以此聚合物作为吸附功能原料制备固相萃取柱,建立固相萃取与液质联用检测农药残留的方法。此方法应用在黄瓜的嘧菌酯、噻虫啉和吡虫啉残留检测上,添加回收率在88.5%94.6%之间,相对标准偏差在1.6%2.9%之间。【结论】该分子印迹聚合物制备较容易,固相萃取柱前处理过程简单,以其为前处理核心与LC-MS/MS仪器建立的农药残留检测方法特异性较好、检测灵敏度较高,具有一定的实用性。