Analytical Method Development and Validation of Phenothrin, Promecarb and Penconazole in Tobacco using Liquid Extraction and Gas Chromatography

Öz

A sensitive method for the determination of phenothrin, promecarb and penconazole residues in tobacco has been developed. Several solvents such as, hexane, ethyl acetate and dichloromethane were tested in order to minimize agricultural products residue. In the study, the best recovery was achieved with dichloromethane. Pesticides residues are extracted from the samples with dichloromethane. Additional clean-up steps are not required for tobacco matrices. Determination and quantification of phenothrin, promecarb and penconazole are performed by gas chromatography-flame ionization detector (GC/FID) and gas chromatography-nitrogen/phosphorus (GC/NPD). The method has been validated for tobacco matrices.  Under the optimum conditions, phenothrin R² value 0.999,   promecarb R² value 0.999, and penconazole R² value 0.999. Limits of determination were 0.008 µg mL^-1 for phenothrin, 0.011 µg mL^-1 for penconazole and 0.007 µg mL^-1 for promecarb. The standard deviations (SDs) levels were in the range 0.01-0.20. Recoveries of phenothrin, promecarb and penconazole from tobacco were found to be higher than 85%. Under this developed method, the concentrations of phenothrin, promecarb and penconazole in the 10 tobacco samples were below the LOD values.

Anahtar Kelimeler

• Tobacco,GC,phenothrin,promecarb,penconazole,liquid extraction

Kaynakça

1. 1. Melgar, M.J, Santaeufemia, M, Garcìa, M.A, Organophosphorus pesticide residues in raw milk and infant formulas from Spanish northwest, Journal of Environmental Science and Health, Part B, 2010, 45, 595–600.
2. 2. Ergonen, A.T, Salacin S, Ozdemir M.H, Pesticide use among greenhouse workers in Turkey. The Journal of Clinical Forensic Medicine, 2005, 12, 205–208.
3. 3. Blair, A, Zahm, S.H, Pearce, N.E, Heineman E.F, Fraumeni J, Clues to cancer etiology from studies of farmers, Scandinavian Journal of Work, Environment and Health, 1992, 18, 209–215.
4. 4. Nicolopoulou-Stamati, P, Maipas, S, Kotampasi, C, Stamatis, P, Hens, L, Chemical Pesticides and Human Health: The Urgent Need for a New Concept in Agriculture, Frontiers Public Health, 2016, 4(148), 1-8.
5. 5. Sun, X.H, Song, J.R., Tan, Z.C, Di, Y.Y, Ma, H.X, Wang, M.H, Sun, L.X, Heat capacity and enthalpy of fusion of penconazole, Thermochimica Acta, 413(1-2), 261-265.
6. 6. Jimenez, J.J, Bernal, J.L, del Nozal, M.J, Toribio, L, Arias, E, Analysis of pesticide residues in wine by solid-phase extraction and gas chromatography with electron capture and nitrogen–phosphorus detection, Journal of Chromatography A, 2001, 919, 147–156.
7. 7. Gelsomino, A, Petrovičowȧ, B, Tiburtini, S, Magnani, E, Felici, M, Multiresidue analysis of pesticides in fruits and vegetables by gel permeation chromatography followed by gas chromatography with electron-capture and mass spectrometric detection, Journal of Chromatography A, 1997, 782, 105-122.
8. 8. Oliva, J, Navarro, S, Barba, A, Navarro G, Determination of chlorpyrifos, penconazole, fenarimol, vinclozolin and metalaxyl in grapes, must and wine by on-line microextraction and gas chromatography, Journal of Chromatography A, 1999, 833, 43–51.

9. 9. Navarro, S, Barba, A, Navarro, G, Vela, N, Oliva, J, Multiresidue method for the rapid determination – in grape, must and wine–of fungicides frequently used on vineyards, Journal of Chromatography A, 2000, 882, 221–229.
10. 10. Arrebola, F.J, Martínez Vidal, J.L, Mateu-Sánchez, M, Álvarez-Castellón, F.J, Determination of 81 multiclass pesticides in fresh foodstuffs by a single injection analysis using gas chromatography–chemical ionization and electron ionization tandem mass spectrometry, Analytica Chimica Acta, 2003, 484, 167–180.
11. 11. Pan, H.J, Ho, W.H, Determination of fungicides in water using liquid phase microextraction and gas chromatography with electron capture detection, Analytica Chimica Acta, 2004, 527, 61–67.
12. 12. Hirahara, Y, Tsumura, Y, Nakamura, Y, Tonogai, Y, Shibata, T, Analysis of Phenothrin and Its Metabolite 3-Phenoxybenzoic Acid (PBA) in Agricultural Products by GC and lon-Trap GC/MS, Journal of Food Protection, 1997, 60(3), 305-309.
13. 13. Sakaue, S, Kitajima, M, Doi, T, High Performance Liquid Chromatographic Determination of d-Phenothrin (Sumithrin®) in Shampoo, Agricultural and Biological Chemistry, 1985, 49(9), 2787-2789.
14. 14. Pacioni, N.L, Veglia, A.V, Determination of poorly fluorescent carbamate pesticides in water, bendiocarb and promecarb, using cyclodextrin nanocavities and related media, Analytica Chimica Acta, 2007, 583, 63–71.
15. 15. Sicbaldi, F, Sarra, A, Copeta, G.L, Diatomaceous earth-assisted extraction for the multiresidue determination of pesticides, Journal of Chromatography A, 1997, 765, 23-30.
16. 16. Millȧn, S, Sampedro, M.C, Unceta, N, Goicolea, M.A, Rodriguez, E, Barrio, R.J, Coupling solid-phase microextraction and high-performance liquid chromatography for direct and sensitive determination of halogenated fungicides in wine, Journal of Chromatography A, 2003, 995, 135–142.
17. 17. Ferrer, I, Thurman, E.M, Liquid chromatography time-of-flight mass spectrometry:principles, tools, and application for accurate mass analysis, John Wiley & Sons, Inc, 2009, 280 p., pp. 251.
18. 18. Pang, G.F, Analytical Methods for Food Safety by Mass Spectrometry: Volume I Pesticides, Academic Press, 2018, 880 p., pp. 43.
19. 19. Lunn, G, HPLC Methods for Recently Approved Pharmaceuticals, John Wiley & Sons, Inc., 2005, pp. 26.
20. 20. Loper, B.L, Anderson, K.A, Determination of pyrethrin and pyrethroid pesticides in urine and water matrixes by liquid chromatography with diode array detection, Journal of AOAC International, 2003, 86(6), 1236-1240.