食品中农药残留分析的样品前处理技术进展

本文综述了近年来食品中农药残留分析的样品前处理技术，重点对超临界流体萃取法在食品农药残留分析中的应用及其联用技术进行了评述；同时对固相微萃取、微波辅助萃取和凝胶渗透色谱法进行了总结。对食物中农药残留分析技术的发展方向进行了讨论。     

粮油作物及茶叶中农药多残留检测的前处理技术进展

综述了粮油作物和茶叶中农药多残留检测的前处理技术,包括超临界流体萃取、加速溶剂萃取、搅拌棒吸附萃取、分散固相萃取、固相微萃取和在线凝胶渗透色谱等样品前处理方式,并详细介绍了各种方法的原理、优点及适用范围,可为粮油作物和茶叶中农药多残留检测技术的发展提供参考。     

样品前处理-色谱在线分析农药残留的研究进展

农药残留分析的样品来源多样、基体复杂,而传统的离线样品前处理中,萃取、转移、净化、浓缩等步骤分步进行,繁琐费时、样品损失较大、精密度和重现性差,因此,发展样品前处理-色谱在线分析技术可望解决这些问题。本文综述了近年来固相萃取、固相微萃取、基质固相分散萃取、膜萃取、微波辅助萃取、加速溶剂萃取和超临界萃取等样品前处理-色谱在线分析农药残留的研究进展,并展望了其应用前景和发展方向。引用文献54篇。     

鸡肉中兽药残留检测技术研究进展

鸡肉中兽药残留检测是食品安全检测关注的热点,作为目前普遍发展的样品前处理技术,超临界流体萃取、加速溶剂萃取、毛细管固相微萃取及其与色谱质谱联用检测兽药残留受到广泛关注。以鸡肉为主要检测基质对这些新技术的基本原理、特点及在兽药残留分析中的应用进行了综述,同时对兽药残留分析的研究方向进行了展望。     

水和食品中有机磷农药残留检测的研究进展

综述了水和食品中有机磷农药残留检测中样品的前处理方法 (包括液液萃取、固相萃取、液相微萃取、固相微萃取、拌棒吸附萃取、磁固相萃取、QuEChERS等)和测定方法(包括气相色谱法、气相色谱-质谱法、液相色谱法、液相色谱-质谱法等)的研究进展(引用文献58篇)。     

兽药残留分析中样品前处理技术研究进展

样品前处理是兽药残留分析中的关键步骤,直接影响检测的结果.近年来,出现了一些新的样品前处理技术,如固相萃取、基质固相分散萃取、固相微萃取、搅拌棒吸附萃取、膜萃取、液相微萃取、超临界流体萃取、加速溶剂萃取、分子印迹、微波辅助萃取.这些技术能够有效地减少分析过程中由样品前处理过程带来的误差,具有前处理快速、简便的优点,同时可与分析仪器联用,实现分析的自动化.本文对这些新技术的基本原理、特点及在兽药残留分析中的应用进行了综述,并对样品前处理的前景进行了展望.     

固相萃取技术在食品痕量残留和污染分析中的应用

食品痕量残留和污染分析中,样品的前处理极为重要,也是其难点所在。由于食品和农产品样品的多样性和复杂性,目前还没有一种前处理技术能够适合所有情况下的所有样品。本文对近年来发展起来的新型固相萃取技术如固相微萃取、搅拌棒吸附萃取、基质固相分散萃取、分子印迹固相萃取、免疫亲和固相萃取、整体柱固相萃取、碳纳米管固相萃取等在食品痕量残留和污染分析中的应用进行了综述,对未来的发展前景作了展望。     

典型卤代阻燃剂的样品处理技术及分析检测研究进展

卤代阻燃剂被广泛用作油漆、纺织品、电子器件的添加剂,由于其具有挥发性,能渗入并长久存在于环境中,在环境和食物链中积累,对人类和其他生物健康造成危害,现已被禁止或限制使用。因此,急需建立更加灵敏、准确的卤代阻燃剂残留分析方法。本文系统介绍了卤代阻燃剂的污染途径,以及近年来关于卤代阻燃剂残留样品前处理方法和检测技术,污染途径包括：土壤、水体、空气、灰尘和生物样品污染途径等;样品前处理方法包括：固相萃取、搅拌棒萃取、分子印迹萃取、磁性固相萃取、超临界流体萃取、加压液体萃取等;检测技术包括：气相色谱-质谱检测法、液相色谱-质谱检测法、免疫分析检测法、X射线荧光法等,并对卤代阻燃剂的分析检测技术进行了总结和展望。     

苹果中5种氨基甲酸酯类农药的超临界流体萃取及其气相色谱法测定

提出了一种采用超临界流体萃取技术对苹果中５种氨基甲酸酯类农药进行萃取及用气相色谱检测的方法。实验以二氧化碳作为超临界流体，加入３％的甲醇作为改性剂，对３种惰性载体和加入硅藻土的苹果基体的超临界萃取条件进行了选择，以气相色谱配以氮磷检测器检测５种氨基甲酸酯类农药，取得了满意的结果，回收率为８８％～９８％。     

苹果中5种氨基甲酸酯类农药的超临界流体萃取及其气相色谱法测定

 提出了一种采用超临界流体萃取技术对苹果中５种氨基甲酸酯类农药进行萃取及用气相色谱检测的方法。实验以二氧化碳作为超临界流体，加入３％的甲醇作为改性剂，对３种惰性载体和加入硅藻土的苹果基体的超临界萃取条件进行了选择，以气相色谱配以氮磷检测器检测５种氨基甲酸酯类农药，取得了满意的结果，回收率为８８％～９８％。     

Determination of pesticides in fruit and fruit juices by chromatographic methods. An overview

In order to combat a variety of pests, pesticides are widely used in fruits. Several extraction procedures (liquid extraction, single drop microextraction, microwave-assisted extraction, pressurized liquid extraction, supercritical fluid extraction, solid-phase extraction, solid-phase microextraction, matrix solid-phase dispersion, and stir bar sorptive extraction) have been reported to determine pesticide residues in fruits and fruit juices. The significant change in recent years is the introduction of the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) methods in these matrices analysis. A combination of techniques reported the use of new extraction methods and chromatography to provide better quantitative recoveries at low levels. The use of mass spectrometric detectors in combination with liquid and gas chromatography has played a vital role to solve many problems related to food safety. The main attention in this review is on the achievements that have been possible because of the progress in extraction methods and the latest advances and novelties in mass spectrometry, and how these progresses have influenced the best control of food, allowing for an increase in the food safety and quality standards.     

A review of sample preparation methods for the pesticide residue analysis in foods

The pesticide residues in foods have received increasing attention as one of the most important food safety issues. Therefore, more strict regulations on the maximum residue limits (MRLs) for pesticides in foods have been established in many countries and health organizations, based on the sensitive and reliable analysis methods of pesticide residues. However, the analysis of pesticide residues is a continuing challenge mainly because of the small quantities of analytes as well as the large amounts of interfering substances which can be co-extracted with them, often leading to experimental errors and damage to the analytical instruments. Thus, extensive sample preparation is often required for the pesticide residue analysis for the effective extraction of the analytes and removal of the interferences. This paper focuses on reviewing the recent development in the sample preparation methods for the pesticide residue analysis in foods since 2006. The methods include: liquid-liquid extraction (LLE), supercritical-fluid extraction (SFE), pressurized-liquid extraction (PLE), microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), gel permeation chromatography (GPC), solid-phase extraction (SPE), molecularly imprinted polymers (MIPs), matrix solid-phase dispersion (MSPD), solid-phase micro-extraction (SPME), QuEChERS, cloud point extraction (CPE) and liquid phase micro-extraction (LPME), etc. Particularly their advantages, disadvantages and future perspectives will be discussed.     

Sample preparation methods in the analysis of pesticide residues in baby food with subsequent chromatographic determination

Pesticides are widely utilized at various stages of cultivation and during postharvest storage to protect plants against a range of pests and/or to provide quality preservation. Reliable confirmatory methods are required to monitor pesticide residues in baby foods and to ensure the safety of baby food supply. This review covers methods in which pesticide residues have been determined in baby food by the use of a wide range of chromatographic techniques after various sample preparation steps. The main attention is paid to the evaluation and improvement of sample extraction and clean-up methods (liquid extraction, solid-phase extraction (SPE), dispersive SPE (DSPE), microextraction procedures, matrix solid-phase dispersion (MSPD) and supercritical fluid extraction (SFE)) considering low concentration levels of pesticide residues in baby food resulting from stringent European Union (EU) legislation. Instrumental aspects together with the matrix effects significantly contributing to the most important parameters considered in pesticide residues analysis of baby food--limits of detection (LODs) and limits of quantification (LOQs) were included within the scope of this overview. Paper involves also monitoring studies.     

Supercritical fluid extraction and quantitative determination of organophosphorus pesticide residues in wheat and maize using gas chromatography with flame photometric and mass spectrometric detection

An automated method using supercritical CO2 and clean-up by solid-phase extraction (SPE) using graphitized carbon black, has been developed for the quantitative determination of organophosphorus pesticide (OPP) residues in wheat and maize. Recoveries were as good as, or better than, those obtained using liquid extraction (LE) and gel permeation chromatography (GPC) for 10 OPP's spiked at levels equivalent to 0.05 and 0.50 microg/g. Lower limits of detection were possible using supercritical fluid extraction (SFE). Incurred residues were found in wheat and maize samples, and good agreement was obtained using SFE+SPE and LE+GPC. The SFE+SPE method required less analyst time and organic solvent, and hazardous waste was reduced.     

Analyses of pesticides and their metabolites in foods and drinks

The importance of matrix pretreatment, sample extraction and clean-up in multiresidue methods for pesticide analyses is discussed, with emphasis on alternative new techniques attempted worldwide such as accelerated solvent extraction, microwave-assisted extraction, solid-phase extraction, solid-phase micro-extraction, matrix solid-phase dispersion, supercritical fluid chromatography, ultrasonic extraction and gel permeation chromatography. Detection employing capillary gas chromatography and high-performance liquid chromatography in conjunction with mass spectrometry, capillary electrophoresis, immunoassay techniques and others is summarized.     

Development of an Analytical Method Based on Accelerated Solvent Extraction, Solid-Phase Extraction Clean-Up, then GC–ECD for Analysis of Fourteen Organochlorine Pesticides in Cereal Crops

A method has been developed for analysis of 14 organochlorine pesticide residues in cereals. After accelerated solvent extraction and solid-phase extraction clean-up on graphitized carbon black/primary–secondary amine (GCB/PSA), to reduce co-extraction of interferences, pesticide residues were analyzed by gas chromatography with electron-capture detection. When the method was validated, recoveries were in the range 78–116%, relative standard deviations were in the range 1.1–16.3%, and limits of detection and quantification were from 1.5 to 4.2 μg kg^?1 and from 4.6 to 12.5 μg kg^?1, respectively.     

Analytical methods for pesticide residues in rice

Rice consumption has increased worldwide over recent decades, as it has become one of the most common foods. Although the analysis of environmental samples coming from rice areas has been well documented, there is less information regarding the analysis of pesticide residues in rice-grain samples.Rice (paddy, brown and white) can be considered a complex matrix, leading to difficulties in the application of the different multiresidue methods described in the literature. This review addresses and compares the principal extraction and clean-up methodologies [e.g., liquid-liquid extraction, solid-phase extraction, pressurized-liquid extraction, QuEChERS (quick, easy, cheap, effective, rugged and safe), gel-permeation chromatography and supercritical-fluid extraction - with QuEChERS-based methods being the most frequently employed].Traditionally, the determination of pesticide residues in rice has been based on gas chromatography with mass spectrometry (MS). But the application of new classes of pesticides has driven laboratories to increase the use of liquid chromatography with tandem MS. The limits of detection and quantification are in the ranges 0.09-90 μg/kg and 1-297 μg/kg, respectively, for the methodologies reported. These values agree with the current internationally-accepted maximum residue limits (MRLs).Based on the European Union (EU) database, more than 3000 analyses of pesticide residues in rice have been performed by official EU laboratories over the past decade. Of these, 6% reported pesticide residues above the MRLs.Physico-chemical properties can explain the occurrence of pesticides in rice commodities: lipophilic pesticides are frequently found in brown rice, whereas fungicides are mainly found in milled rice. Carbendazim, malathion, iprodione, tebuconazole, quinclorac and tricyclazole are the pesticides most frequently found in white rice, while buprofezin, hexaconazole, chlorpyrifos and edifenphos are most commonly found in paddy rice.Pesticide-residue concentrations can be affected during rice processing - with concentrations generally lower in the final products. However, few studies focusing on primary processing have addressed the setting of precise values applicable for the processing factors.     

Evaluation of different sample treatments for determining pesticide residues in fat vegetable matrices like avocado by low-pressure gas chromatography-tandem mass spectrometry

A multi-residue method has been developed for determining 65 pesticide residues in greasy vegetable matrices such as avocado. Conventional organic solvent extraction assisted by a high-speed homogenizer was compared to pressurized liquid extraction (PLE) as extraction techniques. Following this, the lipophilic extract was purified using gel permeation chromatography (GPC). Alternative clean-up methods were also evaluated, as solid-phase extraction cartridges individually used and downstream coupled, but less effective lipophilic separation was archived. The pesticide residue determination was carried out using low-pressure gas chromatography coupled to tandem mass spectrometry (LP-GC-MS-MS), showing the applicability of this type of GC columns for the analysis of fat vegetable matrices. The proposed methodology was validated in avocado matrix. The recoveries were in the range 70-110%, with RSD values lower than 19%, at 12 and 50 microg/kg spiking levels. The limits of quantitation (LOQs) were in the range 0.04-8.33 microg/kg and the limits of detection (LODs) were between 0.01 and 2.50 microg/kg. All of them were lower than the maximum residue levels (MRLs) set by the European Union (EU) in avocado. The proposed method was evaluated analyzing pesticide residues in real avocado samples.     

气相色谱-质谱法分析烟草中有机磷农药残留量及其烟支转移率研究

建立了一种用加速溶剂萃取,自动固相萃取净化,气相色谱/质谱联用检测烟草中29种有机磷农药残留量的方法.考察了加速溶剂萃取仪的萃取温度、溶剂、加热时间和循环次数对回收率的影响,对固相萃取的洗脱溶液及其体积和流速进行了优化,利用保留时间和定性离子定性,以灭蚁灵为内标进行定量,29种有机磷农药的平均回收率在61.4%～128%之间,相对标准偏差在12%以下,符合烟草中农药多残留检测的要求.通过对烟支进行加标,探讨了有机磷农药向主流烟气和烟蒂的转移情况,其向主流烟气的平均转移率为小于6.3%,相对标准偏差为8.0%～18.5%,而烟蒂平均截留率为0.3%～15.0%,相对标准偏差为6.5%～21.3%,表明有机磷农药有较小的转移,为卷烟安全性评价提供了可靠的数据.