Document Detail


Multiresidue determination of organochlorine pesticides and polychlorinated biphenyls in milk by gas chromatography with electron-capture detection after extraction by matrix solid-phase dispersion.
MedLine Citation:
PMID:  11601477     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
A multiresidue analytical method based on matrix solid-phase dispersion was developed to analyze liquid milk for 22 organochlorine pesticides (OCPs) and 6 polychlorinated biphenyls (PCBs). Initial extraction is performed by loading 3 mL milk onto a 2.0 g octadecyl (C18)-bonded silica cartridge with n-hexane as the eluant. Neutral alumina column chromatography with sodium sulfate as the drying agent is used for further cleanup. The eluate is concentrated to 0.5 mL, and target analytes are determined by capillary gas chromatography with electron-capture detection. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of milk samples fortified at 10 and 1 microg/L levels. Average recoveries were between 74 and 106% for all residues except beta-HCH, beta-endosulfan, and endosulfan sulfate. Both repeatability and reproducibility relative standard deviation values were < 22% for all residues. Detection limits ranged from 0.02 to 0.12 microg/L and quantitation limits were between 0.02 and 0.62 microg/L. The proposed analytical method may be used as a fast and simple procedure in routine determinations of OCPs and PCBs in milk.
Authors:
C Yagüe; S Bayarri; R Lázaro; P Conchello; A Ariño; A Herrera
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't    
Journal Detail:
Title:  Journal of AOAC International     Volume:  84     ISSN:  1060-3271     ISO Abbreviation:  J AOAC Int     Publication Date:    2001 Sep-Oct
Date Detail:
Created Date:  2001-10-16     Completed Date:  2002-03-05     Revised Date:  2008-03-17    
Medline Journal Info:
Nlm Unique ID:  9215446     Medline TA:  J AOAC Int     Country:  United States    
Other Details:
Languages:  eng     Pagination:  1561-8     Citation Subset:  IM    
Affiliation:
University of Zaragoza, Veterinary Faculty, Department of Animal Production and Food Science, Spain.
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MeSH Terms
Descriptor/Qualifier:
Animals
Chromatography, Gas
Electrochemistry
Indicators and Reagents
Insecticides / analysis*
Milk / chemistry*
Pesticide Residues / analysis*
Polychlorinated Biphenyls / analysis*
Reference Standards
Reproducibility of Results
Solvents
Chemical
Reg. No./Substance:
0/Indicators and Reagents; 0/Insecticides; 0/Pesticide Residues; 0/Polychlorinated Biphenyls; 0/Solvents

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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