Extraction and Gas Chromatographic Screening of 14 Chlorinated Pesticides in Crayfish (Procambarus clarkii) Hepatopancreas

Lott, Heidi M.; Barker, Steven A.

doi:10.1093/jaoac/76.3.663

Cited by 14 publications

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“…Matrix Solid - Phase Dispersion Extraction. Matrix solid-phase dispersion extraction (MSPD) can be applied to a variety of matrixes. − Analytes with a broad range of polarity ranging from polychlorinated biphenyls 40 and pesticides 39 to sulfonamide and β-lactam antibiotics , can be recovered with sufficient extraction yields. The method allows for a comparatively selective extraction of the analytes of interest, thereby simplifying the subsequent isolation steps .…”

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Extraction and Isolation of Linear Alkylbenzenesulfonate and Its Sulfophenylcarboxylic Acid Metabolites from Fish Samples

1999

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Linear alkylbenzenesulfonate (LAS) is the most widely used synthetic surfactant. In fish, assessment of the environmental risk and investigation of the biotransformation behavior of LAS require compound-specific methods for extraction and isolation of LAS and its biotransformation products, sulfophenylcarboxylic acids (SPC). Matrix solid-phase dispersion (MSPD) extraction with subsequent ion-pair liquid-liquid (IP-LL) partitioning of the extract was a time-efficient sample preparation method for analysis of LAS. The recovery of parent LAS from spiked fish exceeded 70%, and the limit of quantitation ranged around 0.2 mg.kg-1 corresponding to 0.6 mumol.kg-1. In a simultaneous determination of LAS and SPC in fish, the analytes were MSPD extracted in different fractions. The target compounds were separated from the sample matrix by protein precipitation and subsequent isolation of (a) SPC by graphitized carbon black solid-phase extraction of the supernatant and (b) parent LAS by IP-LL partitioning of the pellet obtained after protein precipitation. The recoveries of the model compounds C12-2-LAS and C4-3-SPC were 84 +/- 6 and 65 +/- 11%, respectively. The use of C3-3-SPC as an internal standard corrected for the loss of the biotransformation product during sample workup. The suitability of both methods was demonstrated by analyzing fish containing LAS and SPC incurred during aqueous exposure.

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Extraction and Isolation of Linear Alkylbenzenesulfonate and Its Sulfophenylcarboxylic Acid Metabolites from Fish Samples

1999

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Matrix solid-phase dispersion extraction of organophosphorus and synthetic pyrethroid pesticides in cashew nut and passion fruit

Dórea

Lanças

1999

J. Micro. Sep.

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A multiresidue extraction method based on matrix solid‐phase dispersion (MSPD) and capillary gas chromatography–electron capture detection for quantification of five widely used organophosphorus insecticides (diazinon, malathion, parathion, methidathion, and pyrazophos) and one synthetic pyrethroid (permethrin) in Brazilian fruits is described. Cashew nut and passion fruit are plants native to South America. Capillary gas chromatography with mass selective detection was also utilized to confirm the pesticides through mass spectra. Different parameters were optimized, such as the solid phase and dispersant used, amounts, type of eluant and volume, and sample amount. The best results were obtained using a silica gel cartridge column and Florisil as dispersant. The eluant was ethyl acetate. Analysis of fortified fruit (n=3) shows an average recovery of 101.4% for cashew nut and 97.8% for passion fruit at 0.3–1.0‐mg/kg levels. Detection limits ranged from 0.2 to 0.4 pg for the compounds studied using 1‐g samples. The linearity, repeatability, and recoveries of the method are presented. This MSPD method was compared with solid‐phase extraction (SPE) for cleanup, using an alumina–silica gel (1 : 1) cartridge column and ethyl acetate as eluant. Analysis of fortified fruit (n=3) shows an average recovery of 104.9% for cashew nut and 106.8% for passion fruit at 0.1–0.6‐mg/kg levels. Detection limits ranged from 0.2 to 0.6 pg for the compounds studied using 25‐g samples. The combined use of C18 and silica (or Florisil) makes this extraction system unsuitable for these fruits matrixes. The cleanest extracts are obtained using two polar (Florisil and silica) solid phases. In conclusion, the proposed MSPD method described here can be applied to extract five organophosphorus pesticides and permethrin in 1 g of fruit. It is advantageous because it uses ethyl acetate as the only solvent, is faster and uses less solvent than SPE methods, and requires only small sample sizes. ©1999 John Wiley & Sons, Inc. J Micro Sep 11: 367–375, 1999

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Biological Samples in Environmental Analysis: Preparation and Cleanup

Barker

2000

Encyclopedia of Analytical Chemistry

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The most difficult samples to analyze are those derived from biological sources. The analysis of biological samples requires the ability to extract and isolate a wide range of environmental pollutants from an even wider range of matrices, from simple bacteria to tissues and fluids from humans, from fungi to the complex tissues and structures of the plants and products that compose the food chain. These matrices comprise a variety of cells, connective tissues and fibers, fluids and related materials that introduce literally thousands of different organic and inorganic compounds to every analysis effort. In order to recognize and assess the nature and severity of pollution and its impact on humans as well as the flora and fauna that constitute our environment, highly efficient and selective methods for the extraction and cleanup of such samples must be developed. New developments in analytical science have been brought to bear on this problem, speeding the extraction and analysis process while making the resulting analyses more sensitive and selective. The present article examines the historical approach to the extraction and cleanup of biological samples for the analysis of pollutants, and reviews recent advances in technology and methodology that have proven applicable to this field.

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Extraction and Gas Chromatographic Screening of 14 Chlorinated Pesticides in Crayfish (Procambarus clarkii) Hepatopancreas

Cited by 14 publications

References 0 publications

Extraction and Isolation of Linear Alkylbenzenesulfonate and Its Sulfophenylcarboxylic Acid Metabolites from Fish Samples

Extraction and Isolation of Linear Alkylbenzenesulfonate and Its Sulfophenylcarboxylic Acid Metabolites from Fish Samples

Matrix solid-phase dispersion extraction of organophosphorus and synthetic pyrethroid pesticides in cashew nut and passion fruit

Biological Samples in Environmental Analysis: Preparation and Cleanup

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