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Journal of Chromatography A
Volume 1122, Issues 1-2, 28 July 2006, Pages 7-12
 
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doi:10.1016/j.chroma.2006.04.078    How to Cite or Link Using DOI (Opens New Window)
Copyright © 2006 Elsevier B.V. All rights reserved.

Continuous flow microextraction combined with high-performance liquid chromatography for the analysis of pesticides in natural waters

Yi Hea, Corresponding Author Contact Information, E-mail The Corresponding Author and Hian Kee Leeb, Corresponding Author Contact Information, E-mail The Corresponding Author

aDepartment of Science, John Jay College of Criminal Justice, The City University of New York, 445 W59th Street, New York, NY 10019, USA bDepartment of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore

Received 18 November 2005; 
revised 25 April 2006; 
accepted 26 April 2006. 
Available online 22 May 2006.

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Abstract

Continuous flow microextraction (CFME) combined with high-performance liquid chromatography-ultraviolet (HPLC-UV) detection has been applied to the analysis of five widely used pesticides, simazine, fensulfothion, etridiazole, mepronil and bensulide, present at trace levels in water samples. CFME employs a single organic solvent drop positioned at the tip of a polyether ether ketone (PEEK) tubing, which is immersed in a continuous flowing aqueous sample solution in a 0.5-ml glass chamber. The PEEK tubing acts as the organic drop holder and fluid delivery duct. Analytes are partitioned between the organic drop and the bulk sample solution. Important extraction factors including type of solvent, its volume, sample solution flow rate, extraction time, its pH and addition of salt were investigated. All pesticides exhibit good linearity in the investigated concentration range of 25–250 ng ml−1 with coefficients of determination (R2) ranging from 0.9879 to 0.9999 under the optimized conditions. Detection limits lower than 4 ng ml−1 were obtained for all analytes. The method was evaluated by analyzing natural water sample collected from a reservoir in Singapore. This study for the first time demonstrated the compatibility of CFME procedure and HPLC separation.

Keywords: Continuous flow microextraction; High-performance liquid chromatography; Pesticides; Water analysis

Article Outline

1. Introduction
2. Experimental
2.1. CFME setup and extraction
2.2. Reagent
2.3. HPLC analysis
3. Results and discussion
3.1. Extraction solvent
3.2. Effect of solvent volume
3.3. Effect of flow rate of sample solution
3.4. Effect of extraction time
3.5. Effect of pH value and addition of salt
3.6. Quantitative analysis
3.7. Method application to natural water analysis
4. Conclusion
Acknowledgements
References






 
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