Development of Sample Preparation for Pesticide Residues Analysis in Difficult Food Matrices
Abstract
QuEChERS method has been widely used for pesticide residues analysis in fruits and vegetables because it is found to be quick, easy, cheap and effective. But some fruits and vegetables such as onion, garlic, carrot, and avocado which are complex matrices can cause some particular difficulties for instrumental determination. This article describes the development of extraction and cleanup step of representative pesticides i.e, trans-heptachlor epoxide, chlorpyrifos and cypermethrin in complex matrices sample. For extraction, the main factors (sulfur-containing compounds, pigment and oil) were studied and optimized in experiments to maximize analyze recoveries. Various sample preparation procedures and d-SPE with different sorbents were also investigated to minimize co-extractives and interferences. As the result, in Allium plant, the use of 3% aqueous phosphoric acid blended with frozen samples prior to extraction step was required and for carrot and avocado were treated by standard method. For all commodities, the mixture of MgSO4, PSA, GCB and C18 showed to be much more efficient to remove interferences than the original method. The final selected method was evaluated and compared with U.S. FDA PAM 302 method using both detection techniques (GC-ECD and GC-FPD). The results demonstrated that the method achieved acceptable recoveries of 63.7-119.6% with RSD of 0.8-19.8% at 0.2 mg/kg. This method can be applied for routine analysis of these pesticide residues in onion, garlic carrot and avocado. Keywords : sample preparation, fruits and vegetables, pesticide residues, QuEChERSReferences
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Chamkasem, N., Ollis, L.W., Harmon, T., Lee, S., & Mercer, G. (2013). Analysis of 136 pesticides in avocado using a modified QuEChERS method with LC-MS/MS and GC-MS/MS. J. Agric. Food Chem., 61, 2315-2329.
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Norli, H.R., Christiansen, A.L., & Stuveseth, K. (2016). Analysis of non-cleaned QuEChERS extracts for the determination of pesticide residues in fruit, vegetables and cereals by gas chromatography-tandem mass spectrometry. Food Addit Contam Part A Chem Anal Control Expo Risk Assess., 33(2),
300-12.
Rahman, M.M., Park, J.H., Abd El-Aty, A.M., Choi, J.H, Bae, H.R., Yang, A., Park, K.H., & Shim, J.H. (2013). Single-step modified QuEChERS for determination of chlorothalonil in shallot (Allium ascalonicum) using GC-μECD and confirmation via mass spectrometry. Biomed Chromatogr., 27(4), 416-21.
U.S. Food and Drug Administration. (1994). Pesticide Analytical Manual Vol. I, Multiresidue Methods, (3rd Ed), Washington DC: U.S. Department of Health and Human Services.
Wilkowska, A., & Biziuk, M. (2011). Determination of pesticide residues in food matrices using the QuEChERS methodology. Food Chemistry, 125, 803–812.
Wittayanan, W. & Chaimongkol T. (2018). Method development of simultaneous determination of organophosphorus and synthetic pyrethroid pesticide residues in some food by gas chromatographic technique. Bull Dept Med Sci, 60(1), 29-44.
Wittayanan, W., Chaimongkol, T., & Jongmevasna, W. (2017). Multiresidue method for determination of 20 organochlorine pesticide residues in fruits and vegetables using modified QuEChERS and GC-ECD/GC-MSD. International Food Research Journal, 24(6), 2340-2346.
Chamkasem, N., Ollis, L.W., Harmon, T., Lee, S., & Mercer, G. (2013). Analysis of 136 pesticides in avocado using a modified QuEChERS method with LC-MS/MS and GC-MS/MS. J. Agric. Food Chem., 61, 2315-2329.
Gaithersburg, M.D. (2007). Pesticide residues in foods by MeCN extraction and partitioning with magnesium sulfate. Official Methods of Analysis of AOAC International. AOAC International, Method 2007.1.
Norli, H.R., Christiansen, A.L., & Stuveseth, K. (2016). Analysis of non-cleaned QuEChERS extracts for the determination of pesticide residues in fruit, vegetables and cereals by gas chromatography-tandem mass spectrometry. Food Addit Contam Part A Chem Anal Control Expo Risk Assess., 33(2),
300-12.
Rahman, M.M., Park, J.H., Abd El-Aty, A.M., Choi, J.H, Bae, H.R., Yang, A., Park, K.H., & Shim, J.H. (2013). Single-step modified QuEChERS for determination of chlorothalonil in shallot (Allium ascalonicum) using GC-μECD and confirmation via mass spectrometry. Biomed Chromatogr., 27(4), 416-21.
U.S. Food and Drug Administration. (1994). Pesticide Analytical Manual Vol. I, Multiresidue Methods, (3rd Ed), Washington DC: U.S. Department of Health and Human Services.
Wilkowska, A., & Biziuk, M. (2011). Determination of pesticide residues in food matrices using the QuEChERS methodology. Food Chemistry, 125, 803–812.
Wittayanan, W. & Chaimongkol T. (2018). Method development of simultaneous determination of organophosphorus and synthetic pyrethroid pesticide residues in some food by gas chromatographic technique. Bull Dept Med Sci, 60(1), 29-44.
Wittayanan, W., Chaimongkol, T., & Jongmevasna, W. (2017). Multiresidue method for determination of 20 organochlorine pesticide residues in fruits and vegetables using modified QuEChERS and GC-ECD/GC-MSD. International Food Research Journal, 24(6), 2340-2346.
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Published
2018-10-02
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