European Journal of Chemistry

A quick method for surveillance of 59 pesticide residues in fruits and vegetables using rapid three-dimensional gas chromatography (GC/MSD/µ-ECD/FPD) and LC/MS-MS

Main Article Content

Gouri Satpathy
Yogesh Kumar Tyagi
Rajinder Kumar Gupta


This article describes a simple, quick and inexpensive method for determination of pesticides in fruits and vegetables. The method, known as the quick, easy, cheap, effective, rugged and safe (QuEChERS) method for pesticide residues, involves the extraction and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate (MgSO4) plus sodium acetate (NaAc) followed by a simple cleanup step known as dispersive solid-phase extraction (dSPE). The extracts were analyzed by three-dimensional gas chromatography GC/MSD/µ-ECD/FPD in trace ion mode and liquid chromatography/tandem mass spectrometry (LC/MS-MS). Method sensitivity, linearity, repeatability and reproducibility, accuracy, matrix effects, and overall uncertainties have been studied for method validation according to the international norm ISO/IEC: 17025:2005 for both techniques. Identification, quantification and reporting with Total and Extracted ion chromatograms, µECD and DFPD were facilitated to a great extent by Deconvolution Reporting Software (DRS) for GC and Mass hunter software for LC. For all compounds LODs were 0.001 to 0.01 mg/kg and LOQs were 0.005 to 0.020 mg/kg. Correlation coefficients of the calibration curves were >0.991.To validate the effects of matrices, repeatability, reproducibility, recovery and overall uncertainty were calculated for twenty-four matrices at 0.020, 0.050 and 0.500 mg/kg. Recovery ranged between 75-107 % with RSD <17 % for repeatability and intermediate precision and UM of ± 13-22 %.


icon graph This Abstract was viewed 2617 times | icon graph Article PDF downloaded 1137 times icon graph Article SUPPLEMENTARY FILE downloaded 0 times

How to Cite
Satpathy, G.; Tyagi, Y. K.; Gupta, R. K. A Quick Method for Surveillance of 59 Pesticide Residues in Fruits and Vegetables Using Rapid Three-Dimensional Gas Chromatography (GC MSD µ-ECD FPD) and LC MS-MS. Eur. J. Chem. 2011, 2, 524-534.

Article Details

Crossref - Scopus - Google - European PMC

[1]. Jaleel, C. A.; Gopi, R., Manivannan, P.; Panneerselvam, R. Pest Biochem. Physiol. 2008, 91, 170-174.

[2]. Stoppelli, I. M.; Crestana, S. Environ. Int. 2005, 31, 731-738.

[3]. Salameh, P.; Waked, M.; Baldi, I.; Brochard, P.; Saleh, B. A. J. Epidemiol. Community Health 2006, 60, 256-261.

[4]. The Prevention of Food Adulteration ACT, 1954 6th Edn. India, 2009.

[5]. Lehotaya, S. J.; Sonb, K. A.; Kwonb, H.; Koesukwiwata, U.; Fud, W.; Mastovskaa, K.; Hoha, E.; Leepipatpiboonc, N. J. Chromatogr. A 2010, 1217, 2548-2560.

[6]. Luke, M. A.; Froberg, J.E.; Masumoto, H. T. J. Assoc. Off. Anal. Chem. 1975, 58, 1020-1026.

[7]. Lee, S. M.; Papathakis, M. L.; Hsiao-Ming, C. F.; Carr, J. E. Fresenius J. Anal. Chem. 1991, 339, 376-383.

[8]. Fillion, J.; Sauve, F.; Selwyn, J. J. AOAC Int. 2000, 83, 698-713.

[9]. Anastassiades, M.; Lehotay, S. J.; Štajnbaher, D.; Schenck, F. J. J. AOAC Int. 2003, 86, 412-431.

[10]. Lehotay, S. J.; Hiemstra, M.; van Bodegraven, P.; de Kok, A. J. AOAC Int. 2005, 88, 595-614.

[11]. Lehotay, S. J.; Mastovska, K.; Lightfield, A. R. J. AOAC Int. 2005, 88, 615-629.

[12]. Lehotay, S. J.; Mastovska, K.; Yun, S. J. J. AOAC Int. 2005, 88, 630-638.

[13]. Tomlin, C. D. S. The Pesticide Manual, 12th edn., The British Crop Protection Council, Farnham, Surrey, UK, 2000.

[14]. Guana, H.; Brewera, W.E.; Garrisb, S.T.; Morgana, S. L. J. Chromatogr. A 2010, 1217, 1867-1874.

[15]. Cook, J.; Beckett, M. P.; Reliford, B.; Hammack, W.; Engel, M. J. AOAC Int. 1999, 82, 1419-1435.

[16]. Mercer, G. E. J. AOAC Int. 2005, 88, 1452-1462.

[17]. Quimby, B.; Szelewski, M. Agilent Application Note 5989-4834EN, Wilmington, DE, 2006.

[18]. Etxebarria, N.; Zuloagaa, O.; Olivaresa, M.; Bartolomea, L.J.; Navarroa, P. J. Chromatogr. A 2009, 1216, 1624-1629.

[19]. Stajnbahera, D.; Zupancic-Kraljb, L. J. Chromatogr. A 2008, 1190, 316-326.

[20]. Mezcua, M.; Martinez-Uroz, M. A.; Wylie, P. L.; Fernandez-Alba, A. R. J. AOAC Int. 2009, 92, 1790-1806.

[21]. Norli, H. R.; Christiansena, A.; Holena, B. J. Chromatogr. A 2010, 13, 2056-2064.

[22]. Agnew, D.; Mata, N.; Weiner, K.; Wylie, P. Agilent Application Note 5968-3433E, Wilmington, DE, 1998.

[23]. Satpathy, G.; Tyagi, Y. K.; Gupta, R. K. Food Chem. 2011, 127, 1300-1308.

[24]. Anastassiades, M.; Lehotay, S. J.; Stajnbher, D.; Schenk, F. J. J. AOAC Int. 2003, 86, 412-431.

[25]. Lehotay, S. J.; De Kok, A.; Hiemstra, M.; Van Bodegraven, P. J. AOAC Int. 2005, 88, 595-614.

[26]. Mastovska, K.; Lehotay, S. J.; Hajslova, J. J Chromatogr A 2001, 926, 291-308.

[27]. NIST (2005), USA

[28]. ISO guide to the expression of uncertainty in measurement (GUM: 1993)). BIPM, IEC, IFCC, ISO, IUPAC, IUPAP, OIML, Geneva.

[29]. Dagan, S. J. Chromatogr. A 2000, 868, 229-247.

[30]. Wylie, P. L.; Szelewski, M. J.; Meng, C. Agilent Application Note 5989-1157EN, Wilmington, DE, 2004.

[31]. ICH-Topic Q2b. (1996). Guidance for industry-Validation of analytical procedures: Methodology. U.S. Department of Health and Human Services.

[32]. Chai, M. K.; Tan, G. H. Food Chem. 2009, 117, 561-567.

Most read articles by the same author(s)

Dimensions - Altmetric - scite_ - PlumX

Downloads and views


Download data is not yet available.


Metrics Loading ...
License Terms

License Terms


Copyright © 2024 by Authors. This work is published and licensed by Atlanta Publishing House LLC, Atlanta, GA, USA. The full terms of this license are available at and incorporate the Creative Commons Attribution-Non Commercial (CC BY NC) (International, v4.0) License ( By accessing the work, you hereby accept the Terms. This is an open access article distributed under the terms and conditions of the CC BY NC License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited without any further permission from Atlanta Publishing House LLC (European Journal of Chemistry). No use, distribution, or reproduction is permitted which does not comply with these terms. Permissions for commercial use of this work beyond the scope of the License ( are administered by Atlanta Publishing House LLC (European Journal of Chemistry).