食品中农药残留检测技术进展

食品农药残留检测的方法可分为常规仪器检测和快速检测.常规的农药残留分析方法如质谱法、气相色谱法、液相色谱法等.常规检测手段不能满足样品现场快速检测的要求,迫使人们运用新的原理和方法去开发特异性强、方便快捷、灵敏度高、准确安全的快速检测新技术.因此,近几年在各个领域展开了农药残留快速检测技术的研究,目前研究和应用较多的农药残留快速检测技术主要是酶联免疫分析法和酶抑制法.     

食用菌农药残留检测方法研究现状探讨

介绍了均质提取、超声提取、加速溶剂萃取、固相萃取净化、凝胶渗透色谱净化和Qu ECh ERS等6种技术在食用菌农药残留检测前处理中的应用,以及气相色谱法和高效液相色谱法两类检测技术在食用菌农药残留检测方面的应用,并比较了各种检测技术方法的优缺点,探讨了食用菌农药残留检测方法的未来发展趋势。     

农药残留的常用分析方法

结合农药残留分析的重要性,主要综述了农药残留检测的常用方法,包括酶抑制法、气相色谱法、气相色谱-质谱法、液相色谱、液相色谱-质谱法,并对农药残留检测的发展前景进行了展望。     

蔬菜农药残留快速检测技术的推广应用

随着我国经济水平的不断提高,农产品生产的重点逐渐从数量转移到质量安全方面。目前,国内农产品质量安全检测的主要是蔬菜中有机磷和氨基甲酸酯类二大类农药残留。国内用于农药残留的常用检测方法有气相色谱法和酶抑制法。气相色谱法成本高,适合用于定性定量检测;酶抑制法操作简便、成本低廉,适合用于定性的快速检测。实现对农产品中蔬菜、水果的农药残留监督,需要推行快速、简便、准确的检测方法,才能达到有效监控的目的。基于此,利用广东省开平市农产品质量监督检测站的技术力量和仪器设备,对目前华南地区占主流地位的4种农药残留快速检测仪器所应用的技术进行了一系列的试验,从而筛选出适用于当前情况的技术,进行推广应用,并调查验证推广应用的效果。     

农药残留快速检测方法研究进展

在果蔬生产中,随着农药的大量和不合理使用,发展相应的农药残留检测技术已越来越受到社会的高度关注和重视,成为全球的焦点。该文概述了近年来果蔬农药残留快速检测方法的研究进展,主要包括酶抑制法、酶联免疫法、生物传感器法、近中红外光谱法、荧光光谱法、拉曼光谱法和核磁共振技术,详细介绍了上述方法的检测原理、研究现状及实际应用情况,分析了各方法的优缺点及研发难点,并对果蔬农药残留快速检测方法的发展趋势进行了展望。     

农产品中农药残留分析技术研究进展

农药残留的极性中毒事件和农产品进出口贸易中农药残留超标问题时有发生,农药残留分析是保证人民群众食品安全和进出口企业利益的重要手段,近年来农产品中农药残留分析技术有了快速的发展。本文主要在农药残留分析中的样品前处理和仪器检测2方面对近5年来的研究进展进行分析和讨论,主要探讨了前处理中的QuEChERS方法的应用、改进和发展,以及仪器检测手段中串联质谱的应用现状及高分辨质谱的应用前景,最后对农药残留分析这两方面的发展进行了展望。     

改进的QuEChERS-液相色谱串联质谱法快速测定中草药中147种农药残留

本文以改进的QuEChERS方法为样品前处理方法,结合液相色谱串联质谱(LC-MS/MS)的检测技术,建立了8种中草药中147种农药残留的检测方法,探究了不同的提取溶剂、除水剂、净化剂的选择和用量的影响。此方法快速、高效,准确度和灵敏度高,适用于中草药中农药多残留的筛查和测定。     

克伦特罗化学发光快速检测系统的验证研究

为了验证克伦特罗化学发光快速检测系统的检测效果,本文用化学发光微粒子免疫法和高效液相色谱法分别对市售猪肉、猪肝、猪尿3种样品中克伦特罗残留量进行检测,比对两种方法试验结果间的差异。结果表明,该快速检测系统对猪肉、猪肝、猪尿3种样品的最低检测限分别为0.25μg/kg、0.23μg/kg、0.17μg/kg;对3种样品做加标回收试验,其回收率在81.5%~102.5%之间,变异系数均小于10%;该系统与高效液相色谱法检测实际样品的检测结果一致。因此,该系统稳定、可靠,可满足食品中克伦特罗残留快速检测的需要。     

鲜果蔬农药残留检测技术研究新进展

主要阐述了近年来果蔬农药残留检测方法的研究新进展,主要包括电子鼻法、电化学传感器法、分子印迹法、近红外光谱法、核磁共振法、气相色谱法在果蔬农药残留检测中的应用现状和发展前景。     

超高效液相色谱法测试分析蔬菜的多种农药残留

通过超高效液相色谱法同时测定蔬菜中吡虫啉、多菌灵、啶虫脒、嘧霉胺和阿维菌素的残留量,确定最佳色谱条件。结果证实,超高效液相色谱法的准确度高、耗时短,特别适用于批量蔬菜样品的农药多残留检测。     

生物传感器在农药残留检测中的应用

农药的广泛使用需要可靠的工具对其进行监测,从而保护人类和环境安全。传统的分析方法由于繁琐耗时或仪器的昂贵有其局限性。生物传感器是一种以生物活性单元为敏感元件,结合化学、物理转换元件,对被分析物具有高度选择性的仪器,可以用来检测农药残留等污染物。该文综述了近年来生物传感器在环境、食品和农产品农药残留检测中的研究进展。     

农药残留的表面增强拉曼光谱快速检测技术研究现状与展望

果蔬农药残留危害人类健康,施药后,农药分布于其表皮和内部组织,果蔬表面农药绝对残留量低、不均匀,直接光谱检测表征难,而表面增强拉曼散射(surface-enhanced Raman scattering,SERS)技术具有分子级检测精度,可以有效扩增信号,在实现微量物质检测方面优势明显。为此,论文综述了国内外表面增强拉曼散射技术的研究现状,特别是详细介绍了通过设计合理的表面增强拉曼基底结构,实现农药残留信号增强的主要技术手段和表面增强拉曼光谱信号分析方法。在此基础上,指出农药残留的表面增强拉曼检测技术研究中的前沿热点问题,探讨并展望了表面增强拉曼技术在农药残留快速检测方面的发展趋势。基于表面增强拉曼的农药高灵敏度、快速检测表征技术,将在农药违禁使用和农药残留超标监管中有广阔应用前景。     

表面增强拉曼光谱检测脐橙果皮混合农药残留

为了研究果皮农药残留快速检测方法。该文以脐橙为例,混合农药(亚胺硫磷和乐果)为研究对象,选用银纳米线作为增强基底,利用共焦显微拉曼光谱仪对农药残留进行检测。通过表面增强拉曼光谱(surface enhanced Raman scattering,SERS)技术,采集脐橙表皮混合农药残留的SERS光谱。对混合农药定性分析,银纳米线对2种农药都有较好的增强效果。对采集的光谱进行预处理后,建立模型,进行定量分析,研究结果表明,经过二阶微分预处理后光谱数据结合偏最小二乘法(partial least squares,PLS)得到的模型预测效果最好,预测相关系数(R_p)为0.954,其预测均方根误差(root-mean-square prediction error,RMSEP)为4.822 mg/L。挑选两种农药特征峰的特征波段,混合农药中亚胺硫磷的特征波段经多元散射校正(multiplicative scatter correction,MSC)处理后,建模效果较好,其中R_p为0.898,RMSEP为6.621 mg/L;混合农药中乐果的特征波段经基线校正处理后,建模效果较好,其中R_p为0.911,RMSEP为7.369 mg/L。研究结果表明SERS技术是一种快速、可靠的检测混合农药残留的方法。     

宁波市鄞州区农作物农药残留现状与控制对策

对鄞州区种植的稻谷、叶菜类、水果类、豆类、茄果类和块茎类农产品按月进行了411个批次抽样,按照国家相关规定对22个农药项目进行了检测。检测结果发现样本农药项目检出率为0.3%,农产品农药残留合格率97.82%,农药残留检出项目中88.89%是杀虫剂。超出农药残留标准的样本主要是5—10月的青菜,叶菜类超标样本率达到3.72%。农药残留超标样本在平原、滨海地区种植散户中有发现,而在山区各规模农户中均有发现。小学文化程度农户样本农药残留超标率高达4.50%,是大学文化程度农户样本农药残留超标率的6.16倍。为了降低鄞州区农作物农药残留率,提出5方面的控制对策。     

Contributions of pesticide residue chemistry to improving food and environmental safety: past and present accomplishments and future challenges

The principles of modern pesticide residue chemistry were articulated in the 1950s. Early authors pointed out the advantages of systematizing and standardizing analytical methods for pesticides so that they could be widely practiced and the results could be reproduced from one laboratory to the next. The availability of improved methods has led to a much more complete understanding of pesticide behavior and fate in foods and the environment. Using methods based largely upon gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled increasingly with mass spectrometry (MS) and MS(n) as the detection tool, residues can be measured at parts per billion levels and below in a variety of food and environmental matrices. Development of efficient extraction and cleanup methods, techniques such as ELISA, efficient sample preparation techniques such as QuEChERS, and automated laboratory and field instrumentation has also contributed to the tools available for use in modern pesticide residue analysis. As a result, great strides have been made in improving food and worker safety and in understanding environmental behavior and fate of pesticides. There are many challenges remaining in the field of pesticide residue chemistry that will continue to stimulate analytical chemists. New chemistries are emerging, often patterned on complex natural products. Analyzing for the parent chemicals and potentially multiple breakdown products will require analytical ingenuity. The development of more sensitive bioassays and knowledge of unintended side effects will challenge residue chemistry as well, as in the case of following the fate of environmental endocrine disruptors associated with some pesticides as well as nonpesticide contaminants from packaging materials and other familiar articles. Continued funding and other resources to ensure better training, international cooperation, and accelerated research and development activities will be a constant need in pesticide residue chemistry as it is for all areas of science that aim to mitigate or eliminate contaminants that can affect human and environmental health and safety.     

用于食品安全检测的生物传感器的研究进展

生物传感器特异性好、分析速度快、成本低，在食品安全检测领域有着重要的应用价值。该文介绍了电化学、光学、压电和量热生物传感器在食品安全检测中的应用，包括致病菌、抗生素残留、生物毒素和农药残留检测，指出了目前研究中需要解决的问题并展望了未来发展方向，认为高灵敏度、集成化、微型化、多功能化等是未来用于食品安全检测的生物传感器的发展趋势和重点方向。它在食品污染物的快速实时及特异性检测方面有着广阔的应用前景。     

Analysis of agricultural residues on tea using d-SPE sample preparation with GC-NCI-MS and UHPLC-MS/MS

This study presents new sample preparation and analytical procedures for the quantification of pesticides on processed tea leaves. The new method includes tea extraction and dispersive solid phase extraction (d-SPE) to prepare gas chromatography (GC) and ultrahigh-performance liquid chromatography (UHPLC)-ready samples, providing a fast and cost-effective solution for time-sensitive industrial analysis to fulfill regulatory requirements. Both GC-negative chemical ionization mass spectrometry (GC-NCI-MS) and UHPLC-tandem mass spectrometry (UHPLC-MS/MS) were employed to produce highly sensitive and reproducible data. Excellent limits of detection (typically below 1 μg/kg for GC and 10 μg/kg for UHPLC), wide linearity ranges, and good recoveries (mostly >70%) were achieved on the selected pesticides. Twenty-seven tea samples purchased from local grocery stores were analyzed using the newly developed methods. Among the pesticides analyzed, endosulfan sulfate and kelthane were the most frequently detected by GC-NCI-MS and imidacloprid and acetamiprid by UHPLC-MS/MS in these teas. The samples were found to be relatively clean, with <1 mg/kg of total pesticide residues. The organic-labeled teas were significantly cleaner than nonorganic ones. The cost per gram of tea did not correlate with pesticide residue levels detected.     

苹果果实中毒死蜱残留的品种间差异及套袋对毒死蜱残留的影响

为探讨苹果果实中毒死蜱残留的品种间差异及套袋对其残留的影响作用,采用气相色谱法（GC-FPD）,研究了不同品种苹果果实中毒死蜱的残留动态以及套袋对苹果果实不同部位中毒死蜱残留的影响。结果表明,毒死蜱在苹果果实中的残留量存在着明显的品种差异,其中红富士属于高农药残留的品种,而嘎拉、红将军和83-1-70-3则属于低农药残留的品种。毒死蜱在苹果果实不同部位中的残留量表现出明显差异,果皮是毒死蜱残留的主要部位,其次是全果,果肉中的残留最少。套袋明显减少了毒死蜱在苹果果实中的残留量,不论处理浓度和取样时间如何,套袋苹果果实中毒死蜱的残留量比不套袋至少减少1/3。     

Tolerance setting process in the U.S. Environmental Protection Agency

The U.S. Environmental Protection Agency (EPA) is responsible for setting tolerances for pesticide residues in food, under the authority of the Federal Food, Drug, and Cosmetic Act. The residue chemistry data required to set tolerances include metabolism in plants and animals, analytical methods, magnitude of the residue, and concentration in processed foods. A key aspect of tolerance-setting procedures is the identity of the residue in the matrix of concern; without knowledge of the chemical moieties that occur as residues, it is impossible to develop suitable methods or generate meaningful residue data. For new chemicals, EPA carries out a single-laboratory validation of the analytical method needed to generate residue data and to enforce tolerances. Tolerance enforcement methods need to be rapid and inexpensive and to use commercially available equipment and reagents. Methods are more complex for many newer pesticides, which are polar compounds that leave low levels of residue. EPA now requires that the registrants of older pesticides, for which methods are not acceptable by today's standards, must develop better methods.