Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography
Science Journal of Analytical Chemistry
Volume 5, Issue 3, May 2017, Pages: 38-45
Received: May 1, 2017;
Accepted: May 8, 2017;
Published: Jul. 4, 2017
Views 2360 Downloads 135
Tesfa Bedassa, Department of Chemistry, Addis Ababa University, Addis Ababa, Ethiopia; Department of Chemistry, Wollega University, Nekemte, Ethiopia
Negussie Megersa, Department of Chemistry, Addis Ababa University, Addis Ababa, Ethiopia
Abera Gure, Department of Chemistry, Addis Ababa University, Addis Ababa, Ethiopia; Department of Chemistry, Jimma University, Jimma, Ethiopia
A salting-out assisted liquid-liquid extraction (SALLE) method followed by high-performance liquid chromatography with ultraviolet-visible detector (HPLC-UV/Vis) has been proposed for determination of five multiclass pesticides residues including, atrazine, ametryn, terbutryn, carbaryl and chlorothalonil from various alcoholic beverages: beer, wine and Ethiopian honey wine (Tej). Experimental parameters influencing the extraction efficiency of the method such as the type and concentration of salt, volume of acetonitrile (the extraction solvent) and pH of the sample were assayed and the optimum conditions were established. Under the optimum experimental conditions, matrix-matched calibration curves were constructed using beer sample as the representative matrix and good linearity over wide concentration ranges were obtained with coefficient of determination (r2) of 0.997 or better. The limits of detection (LOD) and quantification (LOQ) of the method, which were determined as 3 and 10 times a signal-to-noise ratio (S/N), were in the ranges of 1.3-3.9 and 4.5–12.8 μg L-1, respectively. Precisions studied in terms of repeatability and intermediate precision (with-in lab reproducibility) at two concentration levels have demonstrated acceptable %RSD values, which were less than 10% in both cases. The applicability of the method was also investigated by analyzing various alcoholic beverages and demonstrated satisfactory recoveries in the ranges of 71-104% with their corresponding %RSDs less than 10% in all cases. The results of the study revealed that the developed SALLE method is selective and efficient sample preparation procedure prior to quantitative analysis of the target analytes by HPLC-UV/Vis.
Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography, Science Journal of Analytical Chemistry.
Vol. 5, No. 3,
2017, pp. 38-45.
F. E. Ahmed. (2001). Analyses of Pesticides and Their Metabolites in Foods and Drinks. Trends Anal. Chem. 20: 649–66.
M. Lee, M. Regu and S. Seleshe. (2015). Uniqueness of Ethiopian Traditional Alcoholic Beverage of Plant Origin. tella. J. Ethn. Foods 2: 110–114.
A. Gure, F. J. Lara, A. M. García-Campaña, N. Megersa and M. del Olmo-Iruela. (2015). Vortex-assisted Ionic Liquid Dispersive Liquid–Liquid Microextraction for the Determination of Sulfonylurea Herbicides in Wine Samples By Capillary High-Performance Liquid Chromatography. Food Chem. 170: 348–353.
P. Plaza Bolanos, R. Romero-González, A. Garrido Frenich and J. L. Martínez Vidal. (2008). Application of Hollow-fibre Liquid Phase Microextraction for the Multiresidue Determination of Pesticides in Alcoholic Beverages by Ultra-High Pressure Liquid Chromatography Coupled to Tandem Mass Spectrometry. J. Chromatogr. A 1208: 16–24.
J. Martins, C. Esteves, A. Limpo-Faria, P. Barros, N. Ribeiro, T. Simoes, M. Correia and C. Delerue-Matos. (2012). Analysis of Six Fungicides and one Acaricide in Still and Fortified Wines Using Solid-Phase Microextraction-Gas Chromatography/Tandem Mass Spectrometry. Food Chem. 132: 630–636.
P. Jovanov, V. Guzsvány, M. Franko, S. Lazić, M. Sakač, I. Milovanović and N. Nedeljković. (2014). Development of Multiresidue DLLME and QuEChERS Based LC–MS/MS Method for Determination of Selected Neonicotinoid Insecticides in Honey Liqueur. Food Res. Int. 55: 11–19.
J. W. Wong, M. G. Webster, C. A. Halverson, M. J. Hengel, K. K. Ngim and S. E. Ebeler. (2003). Multiresidue Pesticide Analysis in Wines by Solid-Phase Extraction and Capillary Gas Chromatography−Mass Spectrometric Detection with Selective Ion Monitoring. J. Agric. Food chem. 5: 1148–1161.
J. W. Wong, M. G. Webster, D. Z. Bezabeh, M. J. Hengel, K. K. Ngim, A. J. Krynitsky and S. E. Ebeler. (2004). Multiresidue Determination of Pesticides in Malt Beverages by Capillary Gas Chromatography with Mass Spectrometry and Selected Ion Monitoring. J. Agric. Food Chem. 52: 6361–6372.
N. Megersa and S. Kassahun. (2012). A New Selective Liquid Membrane Extraction Method for the Determination of Basic Herbicides in Agro-Processed Fruit Juices and Ethiopian Honey Wine (Tej) Samples. Food Addit. Contam. 29: 789–798.
M. A. Gonzalez-Curbelo, A. V. Herrera-Herrera, L. M. Ravelo-Perez and J. Hernandez-Borges. (2012). Sample-Preparation Methods for Pesticide-Residue Analysis in Cereals and Derivatives. Trends Anal. Chem. 38: 32–51.
Regulation (EC) No. 396/2005 of the European Parliament and of the Council on Maximum Residue Levels of Pesticides in or on Food and Feed of Plant and Animal Origin and Amending Council Directive 91/414/EEC. Official Journal of the European Communities. No. L 70, 16 March 2005, pp. 1–16.
Regulation (EC) No. 149/2008 Amending Regulation (EC) No. 396/2005 of the European Parliament and of The Council by Establishing Annexes II, III and IV Setting Maximum Residue Levels for Products Covered by Annex I Thereto. Official Journal of the European Communities. No. L 58, 1 March 2008, pp. 1–398.
T. Hyötyläinen, T. Tuutijärvi, K. Kuosmanen and M. L. Riekkola. (2002). Determination of Pesticide Residues in Red Wines with Microporous Membrane Liquid–Liquid Extraction and Gas Chromatography. Anal. Bioanal. Chem. 372: 732–736.
T. Hyötyläinen, K. Lüthje, M. Rautiainen-Rämä and M. L. Riekkola. (2004). Determination of pesticides in red wines with on-line coupled microporous membrane liquid-liquid extraction-gas chromatography. J. Chromatogr. A 1056: 267–271.
J. J. Jimenéz, J. L. Bernal, M. J. del Nozal, L. Toribio and E. Arias. (2001). Analysis of Pesticide Residues in Wine by Solid-Phase Extraction and Gas Chromatography with Electron Capture and Nitrogen-Phosphorus Detection. J. Chromatogr. A 919: 147–156.
G. Cinelli, P. Avino, I. Notardonato and M. V. Russo. (2014). Ultrasound-Vortex-Assisted Dispersive Liquid–Liquid Microextraction Coupled with Gas Chromatography with a Nitrogen–Phosphorus Detector for Simultaneous and Rapid Determination of Organophosphorus Pesticides and Triazines in Wine. Anal. Methods 6: 782–790.
N. Chen, H. Gao, N. Ye, Q. Zhong, Z. Xiong and X. Gu. (2012). Fast Determination of 22 Pesticides in Rice Wine by Dispersive Solid-Phase Extraction in Combination with GC-MS. Am. J. Anal. Chem. 3: 33–39.
A. Economou, H. Botitsi, S. Antoniou and D. Tsipi. (2009). Determination of Multi-Class Pesticides in Wines by Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry. J. Chromatogr. A 1216: 5856–5867.
N. Vela, G. Pérez, G. Navarro and S. Navarro. (2007). Gas Chromatographic Determination of Pesticide Residues in Malt, Spent Grains, Wort and Beer with Electron Capture Detection and Mass Spectrometry. J. AOAC Int. 90: 544–549.
M. J. Hengel, D. Miller and R. Jordan. (2016). Development and Validation of a Method for the Determination of Pesticide Residues in Beer by Liquid Chromatography–Mass Spectrometry. J. Am. Soc. Brew. Chem. 74: 49–52.
M. Ashenafi. (2006). A review on the Microbiology of Indigenous Fermented Foods and Beverages of Ethiopia. Ethiop. J. Biol. Sci, 5: 189–245.
T. Yohannes, F. Melak and K. Siraj. (2013). Preparation and Physicochemical Analysis of Some Ethiopian Traditional Alcoholic Beverages. Afr. J. Food Sci. 7: 399–403.
P. Helena and Z. K. Locija. (1999). Solid-Phase Microextraction. Trends Anal. Chem. 18: 272-282.
I. M. Valente, L. M. Goncalves and J. A. Rodrigues. (2013). Another Glimpse Over the Salting-Out Assisted Liquid-Liquid Extraction in Acetonitrile/Water Mixtures. J. Chromatogr. A 1308: 58–62.
I. M. Valente and J. A. Rodrigues. (2016). Determination of α-Dicarbonyls in Wines Using Salting-Out Assisted Liquid-Liquid Extraction. LCGC 34: 32–37.
A. Jain, M. Gupta and K. K. Verma. (2015). Salting-out Assisted Liquid-Liquid Extraction for the Determination of Biogenic Amines in Fruit Juices and Alcoholic Beverages after Derivatization with 1-Naphthylisothiocyanate and High Performance Liquid Chromatography. J. Chromatogr. A 1422: 60–72.
H. Dong, X. Guo, Y. Xian, H. Luo, B. Wang and Y. Wu. (2015). A salting out-Acetonitrile Homogeneous Extraction Coupled with Gas Chromatography-Mass Spectrometry Method for The Simultaneous Determination of Thirteen N-Nitrosamines in Skin Care Cosmetics. J. Chromatogr. A 1422: 82–88.
X. Xiong and L. Yang. (2015). Salting-out-Assisted Liquid–Liquid Extraction with Acetonitrile for the Determination of Trimetazidine in Rat Plasma Using Liquid Chromatography-Mass Spectrometry. Biomed. Chromatogr. 29: 268–274.
K. Hajkova, B. Jurasek, D. Sykora, T. Palenicek, P. Miksatkova and M. Kuchar. (2016). Salting-out-Assisted Liquid–Liquid Extraction as a Suitable Approach for Determination of Methoxetamine in Large Sets of Tissue Samples. Anal. Bioanal. Chem. 408: 1171–1181.
J. Liu, M. Jiang, G. Li, L. Xu and M. Xie. (2010). Miniaturized Salting-out Liquid–Liquid Extraction of Sulfonamides from Different Matrices. Anal. Chim. Acta 679: 74–80.
H. Sereshti, M. Khosraviani and M. S. Amini-Fazl. (2014). Miniaturized salting-out Liquid–Liquid Extraction in a Coupled-Syringe System Combined with HPLC–UV For extraction and Determination of Sulfanilamide. Talanta 121: 199–204.
D. Jain, R. Athawale, A. Bajaj, and S. Shrikhande (2014). Double-salting out Assisted Liquid–Liquid Extraction (SALLE) HPLC Method for Estimation of Temozolomide from Biological Samples. J. Chromatogr. B 970: 86-94.
S. Ahmed and A. M. Mahmoud. (2015). A Novel Salting-out Assisted Extraction Coupled with HPLC- Fluorescence Detection for Trace Determination of Vitamin K Homologues in Human Plasma. Talanta 144: 480–487.
S. Song, E. N. Ediage, A. Wu and S. De Saeger. (2013). Development and Application of Salting-out Assisted Liquid/Liquid Extraction for Multi-Mycotoxin Biomarkers Analysis in Pig Urine with High Performance Liquid Chromatography/Tandem Mass Spectrometry. J. Chromatogr. A 1292: 111–120.
D. Moreno-González, R. Rodríguez-Ramírez, M. del Olmo-Iruela and A. M. García-Campaña. (2017). Validation of a New Method Based on Salting-out Assisted Liquid-Liquid Extraction and UHPLC-MS/MS for the Determination of Betalactam Antibiotics in Infant Dairy Products. Talanta. 167: 493–498.
Y. Wen, J. Li, F. Yang, W. Zhang, W. Liao, C. Li and L. Chen. (2013). Salting-out Assisted Liquid-Liquid Extraction with the Aid of Experimental Design for Determination of Benzimidazole Fungicides in High Salinity Samples by High-Performance Liquid Chromatography. Talanta 106: 119–126.
A. Gure, F. J. Lara, D. Moreno-González, N. Megersa, M. del Olmo-Iruela and A. M. García-Campaña. (2014). Salting-out Assisted Liquid-Liquid Extraction Combined with Capillary HPLC for The Determination of Sulfonylurea Herbicides Iin Environmental Water and Banana Juice Samples. Talanta 127: 51–58.
X. Y Xu, J. Ye, J. Nie, Z. G. Li and M. R. Lee. (2015). New Liquid–Liquid Microextraction Method by Ultrasound Assisted Salting-out for Determination of Triazole Pesticides in Water Samples Coupled by Gas Chromatography-Mass Spectrometry. Anal. Methods 7: 1194–1199.
S. C. Natina, L. G. Kaldon and D. L. Bailey. (2015). Ammonium Salting-out Extraction with Analyte Preconcentration for Sub-Part per Billion Quantitative Analysis in Surface, Ground and Drinking Water by Flow Injection Tandem Mass Spectrometry. Anal. Methods 7: 2300-2312.
Y. Fan, S. Hu and S. Liu. (2014). Salting-out Assisted Liquid–Liquid Extraction Coupled to Dispersive Liquid–Liquid Microextraction for The Determination of Chlorophenols in Wine by High-Performance Liquid Chromatography. J. Sep. Sci. 37: 3662–3668.
T. Bedassa, A. Gure and N. Megersa. (2015). Modified QuEChERS Method for the Determination of Multiclass Pesticide Residues in Fruit Samples Utilizing High-Performance Liquid Chromatography. Food Anal. Methods 8: 2020–2027.
J. Zhang, H. Wu, E. Kim and T. A. El-Shourbagy. (2009). Salting-out Assisted Liquid/Liquid Extraction with Acetonitrile: A New High Throughput Sample Preparation Technique for Good Laboratory Practice Bioanalysis Using Liquid Chromatography–Mass Spectrometry. Biomed. Chromatogr. 23: 419–425.
A. Tapparo, D. Marton, C. Giorio, A. Zanella, L. Soldà, M. Marzaro, V. Linda and G. Vincenzo. (2012). Assessment of the Environmental Exposure of Honeybees to Particulate Matter Containing Neonicotinoid Insecticides Coming from Corn Coated Seeds. Environ. Sci. Technol. 46: 2592–2599.
R. P. Carneiro, F. A. S Oliveira, F. D. Madureira, G. Silva, W. R. de Souza and R. P. Lopes. (2013). Development and Method Validation for Determination of 128 Pesticides in Bananas by Modified QuEChERS and UHPLC–MS/MS Analysis. Food Cont. 33: 413–423.
Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. European Commission SANTE/11945/2015 Supersedes SANCO/12571/2013, Implemented by 01/01/2016.