国际食品法典加工农产品中农药最大残留限量现状分析

加工农产品中的农药残留信息对于国际贸易及进行更精确的膳食摄入风险评估均非常重要.本文重点介绍了国际食品法典关于制定加工农产品中农药最大残留限量(MRL)和开展膳食摄入风险评估所遵循的一般原则、数据要求、评估方法以及加工农产品分类等信息.国际食品法典委员会目前共制定了586项加工农产品中的农药MRL标准,其中针对谷物碾磨...     

农田尾菜发酵过程中农药残留变化特征

基于尾菜中存在农药残留的现状,以设施农业尾菜黄瓜秧为研究对象,采用气相色谱法和超高效液相色谱-串联质谱法检测了尾菜黄瓜秧在静态好氧发酵过程中多菌灵、吡虫啉、哒螨灵等50种农药残留的动态变化,并分析发酵重要影响因子堆高对农药残留消解的影响。结果表明:在尾菜黄瓜秧中共检测出腐霉利、多菌灵、嘧菌酯、苯醚甲环唑、烯酰吗啉、虫螨腈、吡虫啉、啶虫脒和哒螨灵9种农药残留,其中多菌灵平均残留量最高,达11.2 mg/kg,其他8种农药平均残留量在0.042~0.89 mg/kg之间。在发酵的24 d中,不同堆高条件下9种农药的消解规律均符合一级反应动力学方程,但不同农药半衰期差异较大,其中吡虫啉的平均半衰期最长,为28.9 d,多菌灵的平均半衰期最短,为10.2 d;不同堆高处理中农药的消解速率也有差异,总体上在2.5 m堆高下各农药的消解率最高、半衰期最短。本研究结果可为尾菜发酵参数优化、农业废弃物的高效资源化利用以及研发基于尾菜发酵产物的有机蔬菜专用有机肥提供理论支撑。     

国际食品法典委员会食饲两用商品分类及其农药残留评估现状

本文梳理了国际食品法典委员会(CAC)用于农药残留评估的食饲两用商品的分类，介绍了食饲两用商品中农药残留评估技术及其最大残留限量推荐方法。通过对一个评估实例的剖析，进一步阐明了FAO/WHO农药残留联席会议(JMPR)的评估技术，为提高我国相关领域技术提供借鉴，并基于国内实际提出了建议。     

国际食品法典2015至2019年农药评估优先列表评介

为了解国际食品法典委员会(CAC)农药最大残留限量(MRLs)制定最新动向,文章介绍了2015—2019年CAC的农药评估优先列表,就未来5年内CAC将评估的新化合物、新用途及再评估的化合物进行了总结评述,并对这些化合物在我国的登记情况进行了分析,以供有意向国际食品法典委员会农药残留专家联席会议(JMPR)提交数据的政府或相关企业、以及国内关注国际农药残留限量标准制定进展的相关科研机构参考。同时,文章对我国应如何参与国际残留限量标准制定工作提出了建议,认为我国可通过提交扩大农药使用范围数据,加强我国农药在小作物上的登记,从而促进农产品的出口。     

Organochlorine residues in aquatic environments in Iran, 1974.

Organochlorine pesticide residues in various organisms from different aquatic ecosystems in Iran were investigated in spring 1974. DDT levels were high in fish taken from two rivers in southern Iran, whereas low levels were detected in samples obtained from a freshwater lake in the same area. Fish from two of the reservoirs supplying Tehran with potable water contained moderate levels of DDT. The low residue level in pike collected in the Bandar-Pahlavi Mordab in northwest Iran indicates that only a small amount of organochlorine pesticides used in this area enters the pelagic food chain. Sturgeon collected at different places in the Caspian Sea showed similar accumulations of DDT in the muscles and in the eggs. Polychlorinated biphenyls (PCBs) were detected only in samples of sediment from the drainage systems in Tehran.     

Factors affecting residues of pesticides in tea

This paper presents a discussion on residue behaviour of 17 pesticides on tea, on the basis of the research conducted during the last 20 years. Sunlight photolysis and growth dilution were the most important factors affecting pesticide persistence in the growing tea plant, while vapour pressure played an important role in loss of pesticide residues during tea processing. The percentage of pesticide extracted during the tea infusion process was highly related to water solubility. It is suggested that in studies on pesticide residue behaviour on tea, all the four factors should be considered integrally.     

比例推算法在国际食品法典农药最大残留限量评估中的应用

比例推算是指农药使用剂量与收获后农产品中的农药残留量之间具有一定的比例关系。假定该施药剂量与残留量的比例推算关系独立于作物类型、农药种类和施药方式,则超过临界良好农业规范(cGAP)标签范围±25%的施药剂量所导致的农药残留量将可以按比例进行归一化调整,从而增加了可用于评估农药最大残留限量(MRL)的残留数据。对国际食品法典农药残留委员会(CCPR)将比例推算应用于评估农药MRL的历史背景、制定过程以及最终提交给国际食品法典委员会(CAC)审议的比例推算应用指导原则的具体内容进行了综述,总结了采用比例推算法评估MRL的10项指导原则。使用比例推算法有利于增加评估农药MRL时的残留数据,推进农药MRL标准的制定进程。     

Pesticide residues in soil and foodstuff I. Chlorinated pesticides in cattle feed and milk produced in orchard and non-orchard areas

Milk, hay and silage produced in orchard and non-orchard areas have been analysed for their content of chlorinated pesticides. The residue levels in milk produced in orchard areas were about double those in milk produced in non-orchard areas. The levels in hay were much higher (30% up to sevenfold) in the hay produced in orchard areas and the levels in silage from the two areas showed small differences. Milk collected after cattle had been grazing in an orchard for 3 to 4 days contained 10% more pp′-DDT and 2-, 3-, 7- and 15-fold morepp′-DDE, pp′-TDE and heptachlor epoxide, gamma-BHC and pp′-TDE olefin [1-chloro-2,2-bis(p-chlorophenyl)ethylene], respectively, than did the samples collected one day before the cattle grazed in the orchard.     

QuEChERS-超高效液相色谱-串联质谱法检测花生中4种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测花生中精喹禾灵、毒死蜱、乙草胺和吡虫啉残留的分析方法.样品以纳米氧化锆(Nano-ZrO2)、十八烷基键合硅胶(C18)和多壁碳纳米管(MWCNT)组合进行净化,采用UPLC-MS/MS检测,外标法定量.结果表明:在0.001～0.5 mg/L范围内,4种农...     

我国小麦中农药残留及代谢研究进展

为全面了解小麦中农药残留量水平及代谢状况,合理评价小麦及其产品的质量安全和品质,综述了小麦中常用农药残留、代谢的研究现状及综合治理策略。有机磷类、有机氯类及其他一些常用农药在小麦及其产品中的残留水平较低,均未超过国家相关最大残留限量(MRL)标准;目前针对具有典型代谢产物的农药在小麦体内残留、代谢及转化规律的系统研究很少。提出了应进一步加强立法、建立高效的综合防治体系、继续实施小麦生产过程中农药残留监控、加强小麦流通领域的监督抽查力度等农药残留的综合治理策略,可为农药在小麦上的安全合理使用、提高小麦及其产品的质量安全及品质提供参考。     

Extended summaries: Pesticides group and physicochemical and biophysical panel symposium: The impact of genetic engineering on pest management. Engineering insect resistance into crop plants

Residue levels of organophosphorus, organochlorine and carbarmate insecticides, urea, carbamate and anilide herbicides, carbendazim, fumigants and bromide were determined in home-grown and imported wheat sampled at UK flour mills during the period February 1987 to December 1988. A total of 764 samples was analysed but not all the wheats were tested for all the residues; 140 of 474 samples examined for organophosphorus insecticides contained residues at levels above the reporting limit, 23 of 119 samples contained residues of gamma-HCH, seven of 104 contained carbon tetrachloride and one of 104 contained 1,2-dibromoethane. No residues of urea, carbamate or anilide herbicides, carbendazim, carbaryl or methyl bromide were detected in 32, 40, 44 and 45 samples respectively. Inorganic bromide levels in 45 samples examined were consistent with natural occurrence. Only a single imported wheat was found to contain a residue (of 1,2-dibromoethane) at a level in excess of UK statutory maximum residue levels.     

The effect of the annual use of pesticides on soil microorganisms,pesticide residues in the soil and barley yields

A study has been made of the influence of pesticides used annually on soil microorganisms and crop yields. The persistence of these pesticides in the soil was also investigated. The herbicides MCPA, glyphosate, maleic hydrazide and tri-allate, and the insecticide parathion, were applied on experimental plots on which barley was grown during the years 1973-1981. The fungicide 2-methoxyethylmercury chloride was used every year for dressing the seeds grown in pesticide-treated plots. The pesticide treatments did not affect significantly the numbers of several groups of soil microorganisms. A slight increase was, however, observed in the nitrification activity in the soil. The barley yields were on average higher on pesticide-treated plots than on controls because of successful weed control. Pesticide residues in the soil were generally very low; for example, for parathion they were below 0.02 mg kg^?1 within 11 days, and for MCPA 0.06 mg kg^?1 within 7 days. However, the glyphosate residue was 1.6 mg kg^?1 in the autumn 2 days after the treatment, and the residue settled to a level of 0.2 mg kg^?1 during the following summer. No clear dependence was observed between the residue level and the time between treatment and sampling.     

固相萃取-气相色谱-串联质谱法测定大豆油中126种农药残留

建立了同时测定大豆油中126种农药残留的检测方法.样品经乙腈饱和的正己烷溶解并初次除油后用正己烷饱和的乙腈萃取,于 ?5℃、20000 r/min下离心5 min,Captiva EMR-Lipid固相萃取柱净化,乙酸乙酯复溶后采用气相色谱-质谱联用仪(GC-MS/MS)多反应监测(MRM)模式检测,外标法定量.结果表...     

超高效液相色谱-串联质谱法同时检测大米中15种常用农药的残留

建立一种超高效液相色谱-串联质谱同时检测大米中甲氨基阿维菌素苯甲酸盐等15种常用农药残留的方法,考察了基质效应、提取溶剂种类、提取方法以及不同净化方法对15种农药回收率的影响。样品经V (乙腈) : V (丙酮) : V (水) = 16 : 2 : 2混合溶液匀浆提取,分散固相萃取法净化,电喷雾正离子 (ESI+) 模式电离,多反应监测 (MRM) 模式检测,外标法定量。结果表明:在0.005~1 mg/L范围内,甲氨基阿维菌素苯甲酸盐等15种农药的质量浓度与对应的峰面积间线性关系良好,相关系数 (r) ≥ 0.99;在0.01、0.1、1和4 mg/kg 4个添加水平下,15种农药在大米中的平均回收率在82%~116%之间,相对标准偏差在1.2%~12%之间 (n = 5)。方法检出限为0.000 5~0.005 mg/kg,定量限为0.01 mg/kg。用该方法对上海市郊20个批次的大米样品进行测定,均未检出农药残留超标。该方法操作简单、快速、准确,适用于大米中甲氨基阿维菌素苯甲酸盐等15种常用农药残留的同时检测。     

Comparison of adherence tendencies of pesticide residues sprayed on small-, medium-, and large-sized tomatoes

Crop field trials were conducted to investigate the residues of sprayed pesticides on the different sizes of tomatoes. Pesticide residue data in tomatoes varied due to different locations of the three crop fields selected and/or physicochemical properties of the three pesticides tested. The pesticide residue levels in the medium- and small-sized tomatoes were 1.5 and 2.4 times higher than the level in large-sized tomatoes under similar spray conditions, whereas amount of pesticides adhered per unit surface area were approximately equal among all three sizes of tomatoes. The results of this study suggested that the differences in pesticide residue levels were due to differences in the degree of specific surface area of each tomato size. Resultant residue data of medium-sized tomatoes demonstrated a proportional relationship between pesticide residue levels and the specific surface area of tomatoes.     

The impact of altered herbicide residues in transgenic herbicide-resistant crops on standard setting for herbicide residues

The global area covered with transgenic (genetically modified) crops has rapidly increased since their introduction in the mid-1990s. Most of these crops have been rendered herbicide resistant, for which it can be envisaged that the modification has an impact on the profile and level of herbicide residues within these crops. In this article, the four main categories of herbicide resistance, including resistance to acetolactate-synthase inhibitors, bromoxynil, glufosinate and glyphosate, are reviewed. The topics considered are the molecular mechanism underlying the herbicide resistance, the nature and levels of the residues formed and their impact on the residue definition and maximum residue limits (MRLs) defined by the Codex Alimentarius Commission and national authorities. No general conclusions can be drawn concerning the nature and level of residues, which has to be done on a case-by-case basis. International residue definitions and MRLs are still lacking for some herbicide-crop combinations, and harmonisation is therefore recommended.     

Organophosphorus insecticide residues in virgin Greek olive oil, 1988–1990

Organophosphorus insecticide residues have been monitored for two years in virgin olive oil after dimethoate and fenthion treatments to control the olive fruit fly. No dimethoate residues were detected in any of the samples. For the first and second years, 50% and 21%, respectively, of the samples contained no detectable fenthion residues, while 4% and 6%, respectively had residue concentrations exceeding the Codex Alimentarious Maximum Residue Limit (1 mg kg^?1). The mean concentration was 0·236 mg kg^?1 oil and the estimated daily intake of fenthion 0·0002 mg kg^?1 body weight (Acceptable Daily Intake 0·001 mg kg^?1 body weight). The parent compound was the most important residue in fresh samples, while aged samples contained a higher amount of the metabolite fenthion sulfoxide. The contribution of the oxygen analogues (P= 0 metabolites) of fenthion to the total residue concentration was<5% in most cases.     

三种基质中15种农药及其代谢物的不确定度评估

依据GB 23200.113—2018《食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱-质谱联用法》中的QuEChERS方法,建立了一种气相色谱-串联质谱法(GC-MS/MS)测定茶叶、普通白菜和苹果3种基质中15种农药及其代谢物残留量的数学模型,通过分析测定过程的主要不确定度来源,对各个分量进行评估。结果表明：工作曲线拟合和回收率所引入的不确定度较大,其次为标准溶液配制和样品制备,而测量重复性和仪器引入的不确定度相对较小;不同基质对工作曲线拟合、回收率和测量重复性所引入的不确定度存在一定差异;不匹配基质校正曲线会对部分农药造成一定程度的基质增强或抑制效应。该方法适用于GC-MS/MS法测定植物源性食品中农药残留量的不确定度评估,可为农药残留测量结果的准确性提供科学可靠的依据。     

Monitoring pesticides in agricultural and urban soils of the United States.

Organochlorine pesticides were monitored annually in the major agricultural areas of the United States from 1968 to 1973. Results show that agricultural soils are widely contaminated with low levels of organochlorine residues. Residue concentrations are decreasing as applications of the compounds decrease. Annual monitoring of urban areas since 1969 has demonstrated that urban soils generally have higher pesticide residue concentrations than do agricultural soils in the same locations. High concentrations of mercury, cadmium, and lead have also been observed in urban soils.