Pesticide-residue analysis

P. Van Zoonen, E. A. Hogendoom, G. R. Van der Hoof and R. A. Baumann, Selectivity and sensitivity in coupled chromatographic techniques as applied in pesticide residue analysis . Trends. Anal. Chem. 11 11-17 (1992). 

P. Van Zoonen, Coupled cliromatography in pesticide residue analysis , Sci. Total Environ. 132 105-114(1993). 

E. A. Hogendoorn, C. E. Goewie and P. van Zoonen, Application of HPEC column switching in pesticide residue analysis, Eresenius , ]. Anal. Chem. 339 348-356 (1991). 

The Environmental Protection Agency (EPA) has prepared a manual of pesticide residue analysis dealing with samples of blood, urine, human tissue, and excreta, as well as water, air. soil, and dust. 

For pesticide extraction procedures pertaining to food samples, refer to U.S. government manuals on pesticide residue analysis. 

Egan H. 1969. lUPAC Commission on the development, improvement, and standardization of methods of pesticide residue analysis. J AOAC 52 306-309. 

Stan H-J. 1989. Application of capillary gas chromatography with mass selective detection to pesticide residue analysis. J Chromatogr 467 85-98. 

Shibata Y, Oyama M, Sato H, et al. 1998. Simultaneous cleanup method for multi pesticide residue analysis by GC and HPLC. J Food Hyg Soc Jpn 39(4) 241-250. 

A cadre of analytical agricultural chemists specializing in pesticide residue analysis emerged at a few North American, European and Japanese Universities, regulatory... 

Relationship of pesticide residue analysis, regulation, and risk assessment... 

Komit6 for Levnedsmidler (NMKL)]. The standard presents a universal validation approach for chemical analytical methods in the food sector. This includes methods for the main constituents and also for trace components. Therefore, the NMKL procedure focuses on primary validation parameters, such as specificity, calibration, trueness, precision, LOD or LOQ and does not refer to special requirements of pesticide residue analysis. 

In summary, the procedure of the Nordic Committee describes a comprehensive validation protocol, but it is not specially designed for pesticide residue analysis and has no preferences with regard to single- or inter-laboratory validation. Therefore, if it is applied to pesticide residue methods, some specific validation requirements should be added. The procedure clearly lists all necessary steps of validation and adjusts its recommendations to the degree of previous external validation. 

Ethyl acetate, pesticide residue analysis grade... 

Acetone, acetonitrile, dichloromethane, ethyl acetate, n-hexane and methanol pesticide residue analysis grade... 

Acetone, n-hexane, acetonitrile, ethyl acetate, pesticide residue analysis grade Aluminum oxide, Aluminumoxid 90, activity 11-111, 70-230 mesh MSTM (Merck) Anhydrous sodium sulfate, sodium chloride, special grade Distilled water, HPLC grade... 

Solid-phase sorbents are also used in a technique known as matrix solid-phase dispersion (MSPD). MSPD is a patented process first reported in 1989 for conducting the simultaneous disruption and extraction of solid and semi-solid samples. The technique is rapid and requires low volumes (ca. 10 mL) of solvents. One problem that has hindered further progress in pesticide residues analysis is the high ratio of sorbent to sample, typically 0.5-2 g of sorbent per 0.5 g of sample. This limits the sample size and creates problems with representative sub-sampling. It permits complete fractionation of the sample matrix components and also the ability to elute selectively a single compound or class of compounds from the same sample. Excellent reviews of the practical and theoretical aspects of MSPD " and applications in food analysis were presented by Barker.Torres et reported the use of MSPD for the... 

Capillary electrophoresis (CE) or capillary zone electrophoresis (CZE) is the technique most often employed in pesticide residue analysis. In its most basic form, free zone electrophoresis, a fused-silica capillary is filled with electrolyte (running buffer or background electrolyte). A potential is applied across the capillary and the cations... 

Table 1 Properties of common solvents used in pesticide residue analysis at 20-25 °C...

The most common and diverse approach to cleanup (and extraction of water samples) in pesticide residue analysis is SPE. Over the last 20 years, improvements and diversifications in SPE formats, sorbent types, and apparatus have made SPE a widely used approach for a variety of applications, including the analysis of pesticide residues. SPE cartridges or disks can be likened to low-resolution HPLC columns in that similar stationary and mobile phases are used. A typical particle size in SPE is 40 pm, and the plastic cartridges are generally packed with 0.1-1 g of sorbent in plastic tubes. The choice of reversed-phase, normal-phase, and ion-exchange media in SPE is very diverse, and Table 2 lists some of the more popular SPE applications for the cleanup of pesticides. 

Y. Nakahira, O. Kimura, H. Aoshima, M. Ikeda, Y. Asano, and Y. Yusa, Analysis of the residue of a new fungicide, mepanipyrim, and its metabolites in crops, in Abstracts of the 18th Annual Meeting of the Pesticide Residue Analysis Society of Japan, pp. 1-10 (1994) (in Japanese). 

Distilled water, high-performance liquid chromatography grade Acetone, pesticide residue analysis grade Ethyl acetate, pesticide residue analysis grade n-Hexane, pesticide residue analysis grade Methanol, pesticide residue analysis grade... 

W. Specht, Organochlorine, organophosphorus, nitrogen-containing and other pesticides, S 19, in Manual of Pesticide Residue Analysis (DFG, Deutsche Forschungsgemeinschaft, Pesticides Comm.), ed. H.-P. Their and H. Zeumer, VCH, Weinheim, Vol. 1, pp. 383-400 (1987). 

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