JAST
2012 March;3(1):113-120.
Published online 2011 December 22.
doi:http://dx.doi.org/10.5355/JAST.2012.113
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| Copyright ⓒ 2010 Journal of Analytical Science & Technology |
| In-syringe dispersive liquid-liquid microextraction with liquid chromatographic determination of synthetic pyrethroids in surface water |
| Saeed S. Albaseer1*, R. Nageswara Rao2*, Y. V. Swamy3, K. Mukkanti1 |
1CCST, Institute of Science and Technology, Jawaharlal Technological University Hyderabad Centre for Chemical Sciences and Technology
2*HPLC group, Analytical Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500007, India
3Bioengineering and Environmental Centre, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500007, India |
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Corresponding Author:
R. Nageswara Rao ,Tel: +91-40-2719-3193, Fax: +91-40-2719-3193, Email: rnrao55@yahoo.com |
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ABSTRACT |
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| An indigenously fabricated in laboratory glass syringe was used for in-syringe dispersive liquid-liquid microextraction (is-DLLME) and preconcentration of synthetic pyrethroids (SPs) from surface waters suitable for their determination by high performance liquid chromatography. In contrast to classical DLLME, is-DLLME allows the use of lighter-than-water organic solvents and the analysis of environmental contaminants’ samples without prior filtration, which is of great importance due to the high affinity of pyrethroids to adsorb to solid particulates present in environmental samples. The effects of various parameters on the extraction efficiency were evaluated and optimized systemically using one-factor-at-a-time method (OFAT) and statistically using full factorial design (24). Three SPs (viz.; cypermethrin, resmethrin and permethrin) were analyzed. The method showed good accuracy with RSD% in the range of of 4.8–6.9%. The method detection limits of the three pesticides ranged from 0.14 to 0.16 ng mL-1. The proposed method was applied for the determination of synthetic pyrethroids in lake water |
| Keywords: In-syringe, Dispersive liquid-liquid, Pyrethroids, Lake water, Extraction, HPLC |
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FIGURES |
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Fig.1
Experimental setup of insyringe dispersive liquidliquid microextraction |
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Fig.2
Plot of normalized regression coefficient values, for scaled factors, obtained from MLR, for the three response variables (CYP, RES, PER) studied |
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Fig.3
Plot of linear regression analysis of predicted values by full factorial analysis and experimentally observed values |
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Fig.4
Contour plots for the pyrethroids recovery, as a function of (a) dispersant volume and shaking time and (b) dispersant volume and extraction volume |
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Fig.5
Chromatograms of a: unspiked lake water sample, and b: spiked lake water sample |
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TABLES |
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Table.1
Experimental matrix design of the full factorial design of CYP, RES and PER determinations with is-DLLME. |
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Table.2
ANOVA and results of regression analysis of factorial design for pyrethroids extraction using is-DLLME |
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Table.3
Parameters of quantitative determination of SPs in water by is-DLLME. |
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Table.4
Recoveries and enrichment factors of SPs in water by is-DLLME |
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