Pesticide residue monitoring in Korean agricultural products, 2003–05

Between 2003 and 2005, a total of 11,716 samples were collected and analysed to determine the level of pesticides residues. Multi-residue methods (MRMs) capable of simultaneously determining 250 pesticides were used. Of the 11,716 samples, 89.1% had no detectable residues and 1.7% had violative residues. The detection rates by commodity group were 11.4, 8.6, 0.3, and 0.02% for vegetables, fruit, grain, mushrooms, and the others, respectively. Agricultural products with pesticide residues were pepper, Perilla frutescens, leafy lettuce and spinach in decreasing order. Of the 250 pesticides that were monitored, 70 pesticides were actually found. Procymidone, endosulfan, chlorfenapyr, metalaxyl, and diethofencarb were frequently detected. Of the samples, parsley, Petasites hybridus, Aster scaber and leek had high violative rates of 23.1, 12.6, 8.2, and 7.9%, respectively. From violative samples, procymidone, endosulfan, metalaxyl, diazinon and chlorpyrifos were frequently detected. The violation rates were 1.71, 1.68, and 1.76% in 2003, 2004 and 2005, respectively, and the detection rates were 8.5, 12.0, and 13.3% in 2003, 2004, and 2005, respectively.     

2018年欧盟食品中农药残留情况分析及启示

欧盟向来十分重视食品安全, 在农药残留监管方面, 建立了健全的农药残留监管体系。 本文从欧盟农药残留法规标准、监管部门及分工和欧盟农药残留控制计划3方面介绍了欧盟农药残留监管体系, 从欧盟协调控制计划和国家控制计划两部分分析了2018年欧盟食品中农药残留情况, 涉及样品来源、产品、农药、食品中草甘膦、进口食品、婴幼儿食品、有机食品和动物源性食品等。本文也指出了农药残留产生的原因和风险评估结果, 提出风险管理建议, 并借鉴其监管思路, 提出对我国农药残留监管的几点建议, 为食品安全监管决策提供参考。     

无溶剂萃取技术在食品中农药残留分析的研究进展

无溶剂萃取技术是一种先进的样品制备与前处理技术,常用的有气相萃取、超临界流体萃取、固相萃取、固相微萃取等方法。本文综述了无溶剂萃取技术的基本原理及在食品中农药残留的研究应用进展。     

试纸法快速检测果蔬中有机磷及氨基甲酸酯类农药残留

为了快速检测果蔬中的农药残留,研制基于酶抑制法的农药残留速测试纸。该试纸以鸭血浆胆碱酯酶为检测用酶,2,6-二氯靛酚乙酸酯为底物。反应后根据颜色变化目测判断农药残留情况,强阳性、弱阳性和阴性的颜色分别为白色、浅蓝色和蓝色。用该法检测只需13min,对敌敌畏的敏感性最强,对甲胺磷的敏感性较差,对几种常见的有机磷及氨基甲酸酯类农药的检出限在0.001～6mg/kg之间。该法简便、快速,成本低,适合果蔬中部分农药残留的现场监督检测。     

Determination of pesticide residues in food matrices using the QuEChERS methodology

The determination of pesticide residues in food matrices is a formidable challenge mainly because of the small quantities of analytes and large amounts of interfering substances which can be co-extracted with analytes and, in most cases, adversely affect the results of an analysis. However, safety concerns require that pesticides of the wide range of chemical properties (including acidic, basic and neutral) should be monitored. Because of the wide variety of food matrices, the sample must initially be cleaned up before final analysis. That is why the analytical chemist is faced with the need to devise new methodologies for determining such residues to be determined in a single analytical run. To accomplish the goal, QuEChERS methodology has been developed. It is a streamlined and effective extraction and cleanup approach for the analysis of diverse analyte residues in food matrices. So far, there have been achieved promising results by liquid or gas chromatography analysis, including pesticides, but also acrylamide, pharmaceuticals and veterinary drugs.     

新药创制、环境保护与结构调整--对我国农药工业发展的一点思考

对我国农药工业进行了初步分析,对新药创制、环境保护和农药结构的调整提出了一些建议。     

固相萃取-气相色谱法测定桑葚等浆果中百菌清、腐霉利和联苯菊酯3种农药残留

目的建立固相萃取-气相色谱法测定桑葚等浆果中百菌清、腐霉利和联苯菊酯3种农药残留的分析方法。方法乙腈提取桑葚浆果样品中的3种农药,提取液经HLB固相萃取柱富集、净化,丙酮+环己烷(1:9,V:V)洗脱,洗脱液氮吹至近干,环己烷定容至1 mL,上气相色谱仪定量检测。结果百菌清、腐霉利和联苯菊酯在浓度为0.002～0.200μg/mL范围内线性关系良好;百菌清、腐霉利和联苯菊酯定量限分别为0.0002、0.0006、0.0006 mg/kg;方法加标回收率在85.8%～99.7%之间;精密度和重复性RSD均在10.0%以内。结论方法具有简便、准确、快速等特点,可以用于桑葚等浆果中的农药残留检测。     

固相萃取结合气相色谱法测定蔬菜中33种有机磷农药的残留量

目的建立蔬菜中33种有机磷农药残留量的分析方法。方法蔬菜捣碎后经乙腈提取,盐析,浓缩,SPE柱净化,丙酮定容,采用DB-5MS毛细管柱和FPD检测器测定。可检测33种有机磷农药。结果 33种有机磷农药在40～800μg/L质量浓度范围内呈线性,相关系数(r)为0.998 8～0.999 9。加标回收率为73.1%～108.6%。相对标准偏差(RSD)为1.69%～8.39%。定量检出限3.5μg/kg。结论实验结果表明,在设定色谱条件下用全自动固相萃取仪净化后测定有机磷农药具有简便,快速,灵敏,准确的特点,能满足蔬菜中有机磷农药残留量的检测要求。     

固相萃取-气相色谱-串联质谱法快速监测酸枣仁中有机氯类农药残留

目的建立固相萃取柱净化联合气相色谱-串联质谱法(Carb/NH_2-solid phase extraction-gas chromatography-tandem mass spectrometric, Carb/NH_2-SPE-GC-MS/MS)快速检测79批市售酸枣仁中13种有机氯农药残留,并结合实际污染水平评估有机氯农药的暴露风险。方法样品经乙腈提取,Carb/NH_2SPE柱净化后,采用多离子反应监测模式(MRM)对13种农药残留定量监测。结果13种有机氯农药在5～400μg/kg浓度范围内与对应的峰面积呈现良好的线性关系良好(r~20.996),检出限均低于3μg/kg。本方法应用于79批酸枣仁样品中13种农药的检测,仅1批检出七氯和反式氯丹残留,检出浓度均为0.0025 mg/kg,低于限量规定(0.05mg/kg),慢性暴露风险%ADI为3.95E-03、1.96E-02,表明其无明显健康风险。结论本法操作简单、快速、灵敏度高,可准确监控酸枣仁中有机氯类农药残留。     

拉曼光谱技术在农产品药物残留检测中的应用

近年来,农产品药物残留超标引发了一系列食品安全问题,为了保障国家食品安全、保护消费者健康,需要对农产品中的药物残留进行定性定量检测。表面增强拉曼散射技术 (Surface-enhanced Raman scattering , SERS) 是一种极具吸引力的工具,可用于高效检测农药残留。本文介绍了表面增强拉曼光谱检测技术的概况,简介了拉曼增强基底,分析了表面增强拉曼光谱技术在药物标准溶液、农产品(肉类、水产品、果蔬和其他部分农产品等)药物残留检测领域中的研究现状,并针对当前农产品药物残留检测的发展趋势进行前景展望。