Pesticides multiresidue methods

Garcfa-Reyes, J.F., M.D. Hernando, C. Ferrer, et al. 2007. Large scale pesticide multiresidue methods in food combining liquid chromatography—time-of-flight mass spectrometry and tandem mass spectrometry. Anal. Chem. 79 7308-7323. 

Paya, R, Anastassiades, M., Mack, D., Sigalova, I.,Tasdelen, B., Oliva, J., Barba, A. (2007) Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Analytical and Bioanalytical Chemistry, 389,1697-1714. 

Pubhc concerns about pesticides in the diet of infants and children resulted in an expert committee convened by the U.S. National Academy of Sciences which devoted four years to the review of all available data. A consensus report was issued in 1993 (80). A number of recommendations for further work to more precisely define what constitutes the diet of infants and children were made. No risk could be estimated. The residue data reviewed by the panel were mainly from monitoring studies conducted by the PDA using multiresidue methods to analyze fresh produce and market basket samples collected from various geographic areas (81,82). These and other rehable scientific studies have demonstrated that relatively few food samples contain detectable residues. Most residues are far below estabhshed tolerances which are set above the maximum residue found in treated raw agricultural... 

Pesticide Analytical Manual, Food and Dmg Administration, Rockville, Md., Vol. I, 1990, and Vol. II, 1989. Includes multiresidue methods used by U.S. FDA to routinely check foods for pesticide residues, and single residue methods for certain pesticides not detected by any of the multiresidue methods. 

The U.S. FDA monitors foods for half of the approximately 300 pesticides having official EPA tolerances as weU as a number of other pesticides that have no official tolerances. Multiresidue methods, most of which are based on chromatography protocols, are employed (7). Not aU pesticides are monitored on aU foods and sampling (qv) is purposely biased to catch possible problems. The overaU iacidence of iUegal pesticide residue is, however, quite smaU 1% for domestic surveiUance samples and 3% for imported foods. The methods employed can usuaUy quantify residues present at 0.01 ppm. Quantitation limits range from 0.005 to 1 ppm. 

Chlorophenoxy acids are relatively polar pesticides which are usually determined by LC because volatile derivatives have to be prepared for GC analysis. This group of herbicides can be detected by multiresidue methods combined with automated procedures for sample clean-up, although selectivity and sensitivity can be enhanced by coupled-column chromatographic techniques (52). The experimental conditions for Such analyses are shown in Table 13.1. 

Bennett DA, Chung AC, Lee SM. 1997. Multiresidue method for analysis of pesticides in liquid whole milk. JAOACInt 80(5) 1065-1077. 

FDA. 1994. Pesticide analytical manual, Vol. 1, 3rd edition, Multiresidue methods. Method 302 Method for Nonfatty Foods Method 303 Method II for Nonfatty Foods, Method 304 Method for Fatty Foods. FDA, US Department of Health and Human Services. 

The methods EN 1528 1996 and EN 12393 1998 comprise a range of old multiresidue methods of equal status, which are widely accepted throughout Europe. These are, e.g., the Luke method and the German Deutsche Forschungsgemeinschaft (DFG) methods S8 and S19 ° (all based on extraction with acetone), the Association of Official Analytical Chemists (AOAC) method 970.52 (using acetonitrile extraction and liquid-liquid partition combined with Horisil column cleanup) and the Dutch ethyl acetate extraction combined with GPC. All methods have been subjected to inter-laboratory studies, although not with all pesticide/matrix combinations, which would be impossible to achieve. 

Pesticide Analytical Manual. Volume 1, Multiresidue Methods, third edition, US Food and Drug Administration Washington, DC, Sect. 302 (1994). 

For example, in order to meet the demanding requirements of legislation such as the European Union (EU) Baby Food Directive (Directive 95/5/EC and subsequent revisions), analysts must improve on the scope and sensitivity of multiresidue methods of analysis. This Baby Food Directive, which became effective on 1 July 2002, limits residues of all pesticides to a maximum level of 0.01 mgkg There will also be a banned list of pesticides, annexed to the Directive, which will not permit the use of certain pesticides on crops intended for use in baby food production. As a consequence, food manufacturers often require residue results for raw or primary ingredients within 24 8 h of sample receipt at the laboratory. 

The European drinking water guidelines set a maximum admissible concentration of 0.10 pgL for individual pesticides and their related compounds in drinking water. The recommended methods for oxime carbamates and their metabolites in groundwater and surface water are suitable for detection limits below 0.10 pgL. The first method is the HPLC/lluorescence multiresidue method of de Kok et al The second method is an HPLC/MS/MS method of DuPont Crop Protection which is specific for oxamyl and may be applicable for the analysis of other oxime carbamates in heavily polluted waters. 

FDA. 1994b. 302 and 303 Methods for nonfatty foods. In Pesticides Analytical Manual, 3rd edition, vol. 1 Multiresidue methods. US. Department of Health and Human Services, Food and Drug Administration. 

Krause RT. 1973. Detemiination of several chlorinated pesticides by the AOAC multiresidue method with additional quantitation of perthane after dehydrochlorination Collaborative study. J Assoc Off Anal Chern 56(3)721-727. 

Recent trends in pesticide analysis in food aims for reduced sample pretreatments or simplified methodologies (as QuEChERS approaches), the use of online purification processes, the use of new adsorbents (such as molecular imprinted polymers (MIPs) and nanomaterials) for the extraction and clean-up processes, and focused on the development of large multiresidue methods, most of them based on LC-MS/ MS. In spite of the relevant role of LC-MS/MS, GC-MS-based methods still play an important role in pesticide analysis in food. Despite the development achieved in the immunochemical approaches, the need for multi-residue methods has supported the development and use of instrumental techniques. 

Carvalho JJ, Jeronimo PCA, Goncalves C et al (2008) Evaluation of a multiresidue method for measuring fourteen chemical groups of pesticides in water by use of LC-MS-MS. Anal Bioanal Chem 392 955-968... 

The determination of diazinon in foods is important because this chemical is used as a pesticide on plant crops and, at least in some cases, in pesticide dips for the control of parasitic infestations in animals (Brown et al. 1987 Miyahara et al. 1992). Because animals are exposed to this compound, both via pesticide dips and by ingestion of crops to which diazinon has been applied, some methods have been reported for animal products. The majority of methods, however, deal with the determination of residues in plant products. Most of the analytical methods found that describe the extraction from, and determination of, diazinon residues in various crops (plant materials) were developed as part of multiresidue methods. They are based on homogenization of the sample with an organic solvent (polar or non-polar) the isolation of the residues from this initial extract and, usually, some additional cleanup prior to the analysis of the extract by GC. The most common non-MS modes of detection exploit the... 

Leoni V, Caricchia AM, Chiavarini S. 1992. Multiresidue method for quantitation of organophosphorus pesticides in vegetable and animal foods. J AOAC International 75(3) 511-518. 

Miyahara M, Suzuki T, Saito Y. 1992. Multiresidue method for some pesticides in lanolin by capillary gas chromatography with detection by electron capture, flame photometric, mass spectrometric, and atomic emission techniques. J Agric Fd Chem 40 64-69. 

Seiber JN, Glotfelty DW, Lucas AD, et al. 1990. A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water. Arch Environ Contam Toxicol 19 583-592. 

RT Krause. Multiresidue methods for carbamate pesticides. Emerging Strategies for Pesticide Analysis 5 99-123, 1992. 

The methods most frequently used to monitor for pesticides are high-performance liquid chromatography (HPLC) and gas chromatography (GC) (14,15). On the other hand, multiresidue analytical techniques are preferred to single-residue methods, because multiresidue methods provide the capability to determine different pesticide residues in a single analysis (12,16-18). As... 

A multiresidue method for analyzing 28 common organophosphorus pesticides and three of their main metabolites (paraoxon-ethyl, paraoxon-methyl, and malaoxon) in a variety of crop samples has been developed (59). The use of LC-DAD techniques allowed identification of both organophosphorus pesticides and metabolites by means of standard and spectral comparisons, respectively. A typical chromatogram for fortified apple extract is shown in Figure 4. 

A Di Corcia, M Marchetti. Multiresidue method for pesticides in drinking water using a graphitized carbon black cartridge extraction and liquid chromatographic analysis. Anal Chem 63 580-585,1991. 

BP Ioerger, JS Smith. Multiresidue method for the extraction and detection of organophosphate pesticides and their primary and secundary metabolites from beef tissue using HPLC. J Agric Food Chem 41 303-307, 1993. 

JJ Blaha, PJ Jackson. Multiresidue method for quantitative determination of organophosphorus pesticides in food. J Assoc Off Anal Chem 68 1095-1099, 1985. 

J Slobodnik, MGM Groenewegen, ER Brouwer, H Lingeman, UAT Brinkman. Fully automated multiresidue method for trace level monitoring of polar pesticides by liquid chromatography. J Chromatogr 642 359-370, 1993. 

OP compounds and carbamate are widely used as insecticides, pesticides, and warfare agents [20,21], Detection of pesticides is usually carried out by multiresidue methods (MRMs) of analysis, which are able to detect simultaneously more than one residue and have been developed mainly based on chromatographic techniques. Two groups of MRMs are used (i) multiclass MRMs that involve coverage of residues of various classes of pesticides, and (ii) selective MRMs, which concern multiple residues of chemically related pesticides (e.g., IV-methyl carbamate pesticides (NMCs), carboxylic acids, phenols, etc.). As foods are usually complex matrices all of the pre-analytical steps (matrix modification, extraction, and clean-up) are often necessary. 

Work Item A multiresidue methods for the gas chromatographic determination of pesticide residues ... 

Crescenzi, C., A. Di Corcia, E. Guerriero, and R. Samperi (1997). Development of a multiresidue method for analyzing pesticide traces in water based on solid-phase extraction and electrospray liquid chromatography mass spectrometry. Environ. Sci. Technol., 31 479 188. 

Schulein, J., D. Martens, P. Spitzauer, and A. Kettrup (1995). Comparison of different solid phase extraction materials and techniques by application of multiresidue methods for the determination of pesticides in water by high-performance hquid chromatography (HPLC). Fresenius J. Anal. Chem., 352 565-571. 

Stan, H.-J. (1995a). Analysis of Pesticides in Ground and Surface Water I. Progress in Basic Multiresidue Methods. Chemistry of Plant Protection Series, Vol. 11. Berlin Springer-Verlag. 

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