Pesticides analytical methods

Marsden PJ, Pearson JG, Bottrell DW. 1986. Pesticide analytical methods - general description and quality control considerations. In Perket CL, ed. Quality control in remedial site investigation Hazardous and industrial solid waste testing (ASTM Spec Tech Publ 925). Vol. 5. Philadelphia, PA American Society for Testing and Materials, 198-212. 

Pesticide Analytical Methods in Sweden, Part 1, Rapport 17/98, National Food Administration, Uppsala (1998). 

T. Pihlstrom, B- Kajrap, and A. Valverde, ValidationdataforlSpesticidesincludedinthemulti-residue method for analysis of pesitddes in fruit and vegetable using ethyl acetate extraction, GPC cleanup and GC determination, in Pesticide Analytical Methods in Sweden , Part 1, Rapport 17/98, National Food Administration, Uppsala (1998). 

B92009 Quality Assurance Project Plan for the National Pesticide Survey of Drinking Water Wells Referee Analyses for Analytical Method 2, Organochlorine Pesticides Analytical Method 4, Carbamates Method 5, Methylcarbamates Method 7, Fumigants and Method 9, Nitrate/Nitrite... 

Marsden PJ, Pearson JG, Bottrell DW. 1986. Pesticide analytical methods - general description and quality control considerations. Hazard Ind Solid Waste Test 5 198-212. 

JF Lawrence. High-performance liquid chromatography of pesticides. Analytical Methods for Pesticides and Plant Growth Regulators. New York Academic Press, 1982, pp 3-34. 

The Food and Drug Administration [FDA] Pesticide Analytical Methods Manual QJ and the Environmental Protection Agency [EPA] Manual for Environmental Analysis (2) describe procedures that have been used for many years. Two of the commonly applied techniques are liquid-liquid partitioning and column adsorption chromatography. These approaches are used to isolate lipohilic and moderately polar residues for primary identification and quantitation with GLC. An evaluation of the number of pesticide residues that were satisfactorily analyzed by this approach was published by McMahon and Burke (3). When one looks at the data it can be seen that the highly polar and water soluble residues do not fit into the analytical scheme very well. In an attempt to rectify this problem, FDA is modifying the multiresidue method... 

Seiber, J. N. (1988). Conventional pesticide analytical methods Cun they be improved. In Pesticide Re.tidues in Food Technologie.t for Detection. Office of Technology A.ssessment OTA-F-398. pp. 142-152. U.S. Goverament Priming Office, Washington. DC,... 

Many of these compounds ate highly colored and have found use as dyes and photographic chemicals. Several pharmaceuticals and pesticides are members of this class. An extremely sensitive analytical method for low hydrazine concentrations is based on the formation of a colored azine. They are also useful in heterocycle formation. Several reviews are available covering the chemistry of hydrazones (80,89) and azines (90). 

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. 

T. Cairns and J. Sherma, eds.. Emerging Strategiesfor Pesticide Analysis, CRC Press, Boca Raton, Fla., 1992, 368 pp. From the series Modem Methods of Pesticide Analysis, presents survey of improvements in extraction and cleanup, detailed descriptions of alternative analytical methods, latest appHcations, and up-to-date references. 

C. Tomlin, ed.. The Pesticides Manual A World Compendium, Incorporating the Agrochemicals Handbook, 10th ed.. The British Crop Protection Council and The Royal Society of Chemistry, Crop Protection PubHcations, Cambridge, U.K., 1994. Includes 725 entries by common name in alphabetic order, with chemical stmcture, chemical name(s), molecular formula, CAS Registry Number, physicochemical properties, commercialisation, mode of action, uses, trade names, analytical methods, mammalian toxicology, ecotoxicology, and environmental fate. 

A multiresidue analytical method based on sohd-phase extraction enrichment combined with ce has been reported to isolate, recover, and quantitate three sulfonylurea herbicides (chlorsulfuron, chlorimuron, and metasulfuron) from soil samples (105). Optimi2ation for ce separation was achieved using an overlapping resolution map scheme. The recovery of each herbicide was >80% and the limit of detection was 10 ppb (see Soil chemistry of pesticides). 

Manual of Analytical Methods, J. F. Thompson, Ed. Quality Assurance Section, Chemistry Branch, EPA, Environmental Toxicology Division, Pesticides, Health Effects Research Laboratory, Research Triangle Park, NC 27711. 

Kolpin DW, Goolsby DA, Thurman EM. 1995. Pesticides in near-surface aquifers An assessment using highly sensitive analytical methods and tritium. J Environ Qual 24 1125-1132. 

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. 

Fukuhara K, Takeda M, Uchiyama M. 1977. [Studies on analysis of pesticide residues in foods (XXV) Analytical method for endosulfan in crops.] ShokuhinEiseigakuZasshi 18 149-153. (Japanese)... 

Zweig G, Sherma J. 1972. Thiodan (endosulfan). In Zweig G, Sherma J, eds. Analytical methods for pesticides and plant growth regulators. Vol. VI. Gas chromatographic analysis. New York, NY Academic Press, 511-513. 

Sherma, J. in J. Sherma, G. Zwdg (Eds.), Analytical Methods for Pesticides and Plaid Growth Regulators, Vol. VII, Academic Press, New York, London, 1973. 

N-Nitroso contamination in pesticide products was first reported by D. Fine and co-workers (] ) who had developed a novel and specific analytical method for N-nitroso compounds, called thermal energy analysis. 

Reviews and checks out analytical methods for pesticides submitted by registrants Monitors residues in imported and domestic food, including processed food Monitors residues in meat and poultry Conducts market basket surveys Monitors pesticides in fish and wildlife... 

Owing to the complexity of multi-residue methods for products of animal origin, it is not possible to outline a simple scheme however, readers should refer to methods described in two references for detailed guidance (Analytical Methods for Pesticides in Foodstuffs, Dutch method collection and European Norm EN 1528. ) There is no multi-method specifically designed for body fluids and tissues. The latter matrix can be partly covered by methods for products of animal origin. However, an approach published by Frenzel et al may be helpful (method principle whole blood is hemolyzed and then deproteinized. After extraction of the supernatant, the a.i. is determined by GC/MS. The LOQ is in the range 30-200 ag depending on the a.i.). 

Validation of the analytical methods for food of animal origin has to be performed with milk, egg, meat, and fat. The latter is required only if log Pqav is >3 and metabolism studies indicate significant residues in fat, because in this case it is likely that an MRL will be set. Other tissues such as kidney or liver must be validated only if an MRL is set or proposed for these tissues. The issue of the general necessity of analytical methods for food of animal origin is not addressed in Directive 96/46/EC or SANCO/825/00. At this moment, the Working Group Pesticide Residues proposes an MRL on a case-by-case basis. However, a pragmatic approach is presented in SANCO/825/00. 

Analytical Methods for Pesticide Residues in Foodstuffs, Ministry of Pubhc Health, Welfare and Sport, Amsterdam, 6th edn. (1996). 

The definitions of method detection and quantification limits should be reliable and applicable to a variety of extraction procedures and analytical methods. The issue is of particular importance to the US Environmental Protection Agency (EPA) and also pesticide regulatory and health agencies around the world in risk assessment. The critical question central to risk assessment is assessing the risk posed to a human being from the consumption of foods treated with pesticides, when the amount of the residue present in the food product is reported nondetect (ND) or no detectable residues . 

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