Issue 10, 2014

Use of Doehlert design in the optimization of extraction conditions in the determination of organochlorine pesticides in bovine milk samples by HS-SPME

Abstract

In this study, the extraction of pesticides lindane, heptachlor, aldrin, dieldrin and endrin from milk samples by HS-SPME was investigated followed by separation/detection of these compounds by gas chromatography coupled to an electron capture detector (GC-ECD). Due to the high complexity of milk samples and the hydrophobicity of the studied organochlorine pesticides, the samples were diluted with saturated NaCl solution prior to optimization of the extraction conditions. Dilution tests indicated that a total sample volume of 2 mL (0.5 mL of milk and 1.5 mL of NaCl solution) provided the best chromatographic responses. The fiber coating DVB/Car/PDMS presented the best extraction efficiency towards the target compounds. Optimization was performed using a Doehlert design, and the best conditions were found to be an extraction temperature of 80 °C and an extraction time of 90 min. The HS-SPME mode was used for all extractions from the milk samples. A single fiber, selected during the optimization of fiber coating, was used throughout the study, and no damage on coating was observed. The analytical figures of merit were evaluated, and good results were obtained for the extraction of the target organochlorine pesticides. The percentages of recovery were higher than 75% and the limit of quantitation ranged from 0.5 to 1.2 μg L−1 (for heptachlor and dieldrin, respectively).

Graphical abstract: Use of Doehlert design in the optimization of extraction conditions in the determination of organochlorine pesticides in bovine milk samples by HS-SPME

Article information

Article type
Paper
Submitted
22 ene. 2014
Accepted
08 mar. 2014
First published
10 mar. 2014

Anal. Methods, 2014,6, 3254-3260

Author version available

Use of Doehlert design in the optimization of extraction conditions in the determination of organochlorine pesticides in bovine milk samples by HS-SPME

J. Merib, G. Nardini and E. Carasek, Anal. Methods, 2014, 6, 3254 DOI: 10.1039/C4AY00202D

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements