The Malaysian Journal of Analytical Sciences Vol 12 No 2 (2008): 444 – 450







Chai Mee Kin1* and Tan Guan Huat2


1Dept. of Science and Mathematics, College of Engineering,

Universiti Tenaga Nasional, Km 7, Jalan Kajang-Puchong,

43009 Kajang, Selangor.

2Dept. of Chemistry, Faculty of Science,

Universiti Malaya, Lembah Pantai,

50603 Kuala Lumpur.


*Corresponding author:



Despite the continuing development of solid-phase microextraction (SPME) fiber coatings, their selection presents some difficulties for analytes in choosing the appropriate fiber for a particular application. There are many types of SPME coatings available commercially. The most widely used for determination of pesticide residues in vegetable and fruits are polydimethylsiloxane (PDMS) and polyacrylate (PA). A headspace solid phase microextraction (HS-SPME) procedure using these two commercialized fibers (PDMS and PA) is presented for the determination of selected groups of organochlorine and organophosphorus pesticides. The extraction performances of these compounds were compared using these two fibers. The optimal experimental procedures for the adsorption and desorption of pesticides were determined. An explanation for the extraction differences is suggested based on the different thickness, polarity of the polymeric film of fibers and the different extracting matrices. In addition, the higher detector response of the pesticides after addition of aliquots of water and an organic solvent to the vegetable and fruit samples are also discussed. The SPME fibers were re-usable until a maximum of 120 extractions.  Finally, the optimized procedures were applied successfully for the determination of these compounds in vegetable and fruits samples. Mean recoveries for all pesticides were between 75.0-97% with RSD below 7%.


Keywords: HS-SPME, GC-ECD, GC-MS, pesticide.



1.       J. Beltran, F. J. Lopez, F. Hernandez, 2000, “Solid-phase microextraction in pesticide residues analysis”, J. of Chromatogr. A, 885, 389-404.

2.       J. Pawliszyn, 1997, “Solid-phase microextraction: Theory and Practice” Wiley –VCH.

3.       M. F. Alpendurada, 2000, “Solid-phase microextraction: a promising technique for sample preparation in environmental analysis – Review”, J. of  Chromatogr. A, 889, 3-14.

4.       M. Correia, C. D. Matos, A. Alves, 2000, “Multi-residue methodology for pesticide screening in wines”, J. of Chromatogr. A, 889, 59-67.

5.       J. J. Jimenez, J. L. Bernal, M. J. del Nozal, 1998, “Solid-phase microextraction applied to the analysis of pesticide residues in honey using gas chromatography with electron capture detection”, J. of Chromatogr. A, 829, 269-277.

6.       H. Kataoka, H. L. Lord, J. Pawliszyn, 2000, “Application of solid-phase microextraction in food analysis”, J. of Chromatogr. A, 880, 35-62.

7.       J. Beltran, F. Hernandez, 2001, “Gas chromatography determination of organochlorine and organophosphorus pesticides in human fluids using solid-phase microextraction”, Anal. Chim. Acta, 433, 217-226.

8.       A. Sanusi, V. guillet, M. Montury, 2004, “Advanced method using microwaves and solid-phase microextraction coupled with gas chromatography-mass spectrometry for the determination of pyrethroid residues in strawberries”, J. of Chromatogr. A, 1046, 35-40.

9.       H. Berrada, G. Font, J. C. Molto, 2004, “Application of solid-phase microextraction for determination phenylurea herbicides and their homologous anilines from vegetables “, J. of Chromatogr. A, 1042, 9-14.

10.    M. Fernandez, C. Padron, L. Marconi, S. Ghini, R. Colombo, A. G. Sabatini, 2001, “Determination of organophosphorus pesticides in honeybees after solid-phase microextraction”, J. of Chromatogr. A, 922, 257-265.

11.    M. Correia, C. D, Matos, A. Alves, 2001, “Development of a solid-phase microextraction gas chromatography electron capture detection methodology for selected pesticides in must and wine samples”, Fresenius J. Anal. Chem., 369, 647-651.

12.    A. L. Simplicio, L. V. Boas, 1999, “Validation of a solid-phase microextraction method for the determination of organophosphorus pesticides in fruit and fruit juice”, J. of Chromatogr. A, 833, 35-42.

13.    Y. I. Chen, Y. S. Su, J. F. Jen., 2002,“Determination of dichlorvos by on-line microwave-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography electron capture detection”, J. of Chromatogr. A, 976, 349-355.

14.    M. J. Gonzalez-Rodriguez, F. J. arreola-Liebanas, A. G. Frenich, J. L. Martinez-Vidal, F. J. Sanchez-Lopez, 2005, “Determination of oxadiazon residue by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry”, Anal. Bioanal. Chem., 382, 164-172.

15.    M. M. Mazida, M. M Salleh, H. Osman, 2005, “Analysis of volatile aroma compounds of fresh chilli (capsicum annuum) during stages of maturity using solid-phase microextraction”, J. of food composition and analysis 18, 427-437.

16.    C. Z. Dong, Z. R. Zeng, X. J. Li, 2005, “Determination of organochlorine pesticides and their metabolites in radish after headspace solid-phase microextraction using calix [4] arene fiber”, Talanta 66, 721-727.

17.    M. Sakamoto, T. Tsutsumi, 2004, “Applicability of headspace solid-phase microextraction to the determination of multiclass pesticide in waters”, J. of Chromatogr. A, 1028, 63-74.

18.    D. A. Lambropoulou, T. A. Albanis, 2001, “Optimization of headspace solid-phase microextraction conditions for the determination of organophosphorus insecticides in natural waters”, J. of Chromatogr. A, 922, 243-255.

19.    I. Bras, L. Santos, A. Alves, 2000, “Monitoring organochlorine pesticides from landfill leachates by gas chromatography-electron capture detection after solid-phase microextraction”, J. of Chromatogr. A, 891, 305-311.

20.    J. Beltran, A. Peruga, E. Pitarch, F. J. Lopez, F. Hernandez, 2003, “Application of solid-phase microextraction for the determination of pyrethroid residues in vegetables samples by gas chromatography-mass spectrometry”, Anal. Bioanal. Chem., 376, 502-511.

21.    D. A. Lambropoulou, T. A. Albanis, 2003, “Headspace solid-phase microextraction in combination with gas chromatography – mass spectrometry for the rapid screening of organophosphorus insecticide residues in strawberries and cherries”, J. of Chromatogr. A, 993, 197-203

22.    J. Dugay, C. Miege, M. C. Hennion, 1998, “Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water”, J. of Chromatogr. A, 795, 27-42.


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