Use of the SPME-GC/MS/FID technique as effective alternatives for the determination of organophosphorus pesticide residues

Beatriz E. Jaramillo-Colorado, Héctor Pertuz-Alandette, Flor M. Palacio-Herrera


Organophosphorus pesticides (OPs), are beingwidely used in agriculture, can cause toxic effects to humans and animals. The indiscriminate use of pesticides has generated numerous environmental problems. Especially, in the long term, it can cause serious harm in ecosystems and their associated individuals. The purpose of this investigation was to determine if the milk that is commercialized in the city of Cartagena de Indias has residual concentrations of organophosphorus pesticides. Seven milk samples were analyzed, e.g. six types of pasteurized milk of different brands and one type of raw milk obtained from a herd of the municipality of Maria la Baja, Bolívar, Colombia. The extraction technique used was solid phase microextraction (SPME) in headspace (HS) mode and the methods employed for separation and identification of the compounds were gas chromatography (GC) with flame ionization detector (FID) and mass spectrometry detector (MSD). This method proved advantageous in its application because of its environmentally soundness and facility in application and its confirmed accurate results. Organophosphorus compounds were not detected in the milk samples.


Milk; organophosphorus Pesticides; Extraction; Identification; Quantification


ARMENTA, S.; DE LA GUARDIA, M.: “Green chromatography for the analysis of foods of animal origin”, TrAC Trends in Analytical Chemistry, 80: 517–530, 2016, DOI:

DAGNAC, T.; GARCIA-CHAO, M.; PULLEIRO, P.; GARCIA-JARES, C.; LLOMPART, M.: “Dispersive solid-phase extraction followed by liquid chromatography–tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk”, Journal of chromatography A, 1216(18): 3702–3709, 2009, DOI:

FAO/OMS: Codex Alimentarius International Food Standard, [en línea], 2010, Disponible en:, [Consulta: 28 de agosto de 2016].

FENIK, J.; TANKIEWICZ, M.; BIZIUK, M.: “Properties and determination of pesticides in fruits and vegetables”, TrAC Trends in Analytical Chemistry, 30(6): 814–826, 2011, DOI:

GAZZOTTI, T.; STICCA, P.; ZIRONI, E.; LUGOBONI, B.; SERRAINO, A.; PAGLIUCA, G.: “Determination of 15 organophosphorus pesticides in Italian raw milk”, Bulletin of environmental contamination and toxicology, 82(2): 251–254, 2009, DOI:

GOMES, M.J.; AMAYA, C.A.; WALISZEWSKI, S. M.; COLÍN, S.A.; F. M.M. GARCÍA: “Review Extraction and clean-up methods for organochlorine pesticides determination in milk”, Chemosphere, 92: 233–246, 2013, DOI:

GONZÁLEZ, R.M.J.; LIÉBANAS, F.A.; FRENICH, A.G.; VIDAL, J.M.; LÓPEZ, F.S.: “Determination of pesticides and some metabolites in different kinds of milk by solid-phase microextraction and low-pressure gas chromatography-tandem mass spectrometry”, Analytical and bioanalytical chemistry, 382(1): 164–172, 2005, DOI:

LEDOUX, M.: “Analytical methods applied to the determination of pesticide residues in foods of animal origin. A review of the past two decades”, Journal of chromatography A, 1218(8): 1021–1036, 2011, DOI:

LIN, W.; WEI, S.; JIANG, R.; ZHU, F.; OUYANG, G.: “Calibration of the complex matrix effects on the sampling of polycyclic aromatic hydrocarbons in milk samples using solid phase microextraction”, Analytica chimica acta, 933: 117–123, 2016, DOI:

MINISTERIO DE SALUD PÚBLICA DE COSTA RICA: “Guia de validación para metodos analiticos”, 1998, Disponible en:

NUNEZ, O.; MOYANO, E.; GALCERAN, M.T.: “LC–MS/MS analysis of organic toxics in food”, TrAC Trends in Analytical Chemistry, 24(7): 683–703, 2005, DOI:

PAGLIUCA, G.; GAZZOTTI, T.; ZIRONI, E.; PAVONCELLI, N.; ROSMINI, R.: “Proposal of an analytical method for determination of residues of organophosphorus pesticides in milk by GLC-NPD”, Veterinary research communications, 28(1): 257–259, 2004, DOI:

RODRIGUES, F. de M.; MESQUITA, P.R.; DE OLIVEIRA, L.S.; DE OLIVEIRA, F.S.; MENEZES FILHO, A.; PEREIRA, P.A. de P.; DE ANDRADE, J.B.: “Development of a headspace solid-phase microextraction/gas chromatography–mass spectrometry method for determination of organophosphorus pesticide residues in cow milk”, Microchemical Journal, 98(1): 56–61, 2011, DOI:

SANG, Z.-Y.; WANG, Y.-T.; TSOI, Y.-K.; LEUNG, K.S.-Y.: “CODEX-compliant eleven organophosphorus pesticides screening in multiple commodities using headspace-solid phase microextraction-gas chromatography–mass spectrometry”, Food chemistry, 136(2): 710–717, 2013, DOI:

SANTAEUFEMIA, M.; MELGAR, M.J.; CEPEDA, A.; GARCÍA, M.A.: “Estudio de la contaminación por plaguicidas organofosforados y triazinas en leche procedente de diversas rutas de recogida”, Revista de Toxicología, 23(1): 7–10, 2006.

SELVI, C.; PARAMASIVAM, M.; RAJATHI, D.S.; CHANDRASEKARAN, S.: “Multiresidue analysis of organochlorine pesticides in milk, egg and meat by GC–ECD and confirmation by GC–MS”, Bulletin of environmental contamination and toxicology, 89(5): 1051–1056, 2012, DOI:

SHAKER, E.M.; ELSHARKAWY, E.E.: “Organochlorine and organophosphorus pesticide residues in raw buffalo milk from agroindustrial areas in Assiut, Egypt”, Environmental toxicology and pharmacology, 39(1): 433–440, 2015, DOI:

TOBISZEWSKI, M.; MECHLINSKA, A.; ZYGMUNT, B.; NAMIESNIK, J.: “Green analytical chemistry in sample preparation for determination of trace organic pollutants”, TrAC Trends in Analytical Chemistry, 28(8): 943–951, 2009, DOI:

VALLECILLA, C.; RODRÍGUEZ, N.; RESTREPO, L.F.; LÓPEZ, C.: “Relación entre residuos de clorpirifos en leche y sangre de vacas Holstein y niveles séricos de estradiol y tiroxina”, Revista Electrónica de Veterinaria. REDVET, 11(1): 1–22, 2010, ISSN: 1695-7504.

XU, C.-H.; CHEN, G.-S.; XIONG, Z.-H.; FAN, Y.-X.; WANG, X.-C.; LIU, Y.: “Applications of solid-phase microextraction in food analysis”, TrAC Trends in Analytical Chemistry, 80: 12–29, 2016, DOI:


  • There are currently no refbacks.