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Ligandless Extraction and Determination of Trace Amounts of Lead in Pomegranate, Zucchini and Lettuce Samples after Dispersive Liquid-Liquid Microextraction with Ultrasonic Bath and Optimization of Extraction Condition with RSM Design

Authors: Fariba Tadayon, Elmira Hassanlou, Hasan Bagheri, Mostafa Jafarian


Heavy metals are released into water, plants, soil, and food by natural and human activities. Lead has toxic roles in the human body and may cause serious problems even in low concentrations, since it may have several adverse effects on human. Therefore, determination of lead in different samples is an important procedure in the studies of environmental pollution. In this work, an ultrasonic assisted-ionic liquid based-liquid-liquid microextraction (UA-IL-DLLME) procedure for the determination of lead in zucchini, pomegranate, and lettuce has been established and developed by using flame atomic absorption spectrometer (FAAS). For UA-IL-DLLME procedure, 10 mL of the sample solution containing Pb2+ was adjusted to pH=5 in a glass test tube with a conical bottom; then, 120 μL of 1-Hexyl-3-methylimidazolium hexafluoro phosphate (CMIM)(PF6) was rapidly injected into the sample solution with a microsyringe. After that, the resulting cloudy mixture was treated by ultrasonic for 5 min, then the separation of two phases was obtained by centrifugation for 5 min at 3000 rpm and IL-phase diluted with 1 cc ethanol, and the analytes were determined by FAAS. The effect of different experimental parameters in the extraction step including: ionic liquid volume, sonication time and pH was studied and optimized simultaneously by using Response Surface Methodology (RSM) employing a central composite design (CCD). The optimal conditions were determined to be an ionic liquid volume of 120 μL, sonication time of 5 min, and pH=5. The linear ranges of the calibration curve for the determination by FAAS of lead were 0.1-4 ppm with R2=0.992. Under optimized conditions, the limit of detection (LOD) for lead was 0.062 μg.mL-1, the enrichment factor (EF) was 93, and the relative standard deviation (RSD) for lead was calculated as 2.29%. The levels of lead for pomegranate, zucchini, and lettuce were calculated as 2.88 μg.g-1, 1.54 μg.g-1, 2.18 μg.g-1, respectively. Therefore, this method has been successfully applied for the analysis of the content of lead in different food samples by FAAS.

Keywords: Dispersive Liquid-Liquid Microextraction, central composite design, Food samples, Flame atomic absorption spectrometry

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[1] Y. Wang, S. Gao, X. Zang, J. Li, and J. Ma, “ Graphen-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples,” Anal. Chim. Acta., Vol.716, 2012, pp.112-118.
[2] I. Narin, and M. Soylak, “Enrichment and determination of nickel(ΙΙ), cadmium(ΙΙ), copper(ΙΙ), cobalt(ΙΙ), and lead(ΙΙ) ions in natural waters, table salts, tea and urine samples as pyrrolidine dithiocarbamate chelates by membrane filtration flame atomic absorption spectrometry combination, ” Anal. Chim. Acta., 493, 2003, pp. 205-212.
[3] F. Shah, T. G. Kazi, H. I. Afridi et al., “The influence of environmental exposure on lead concentrations in scalp hair of children in Pakistan,” Ecotoxicology and Environmental Safety., Vol. 74, No. 4, 2011, pp. 727-732.
[4] A. R. Ghiasvand, S. Shadabi, S. Hajipour, A. Nasirian, and H. Sharghi, “A new dispersive liquid-liquid microextraction method followed by direct GF-AAS determination optimized with experimental design and response surface methodology for determination of Ag(ΙΙ) in water samples,” Anal and Bioanal. Chem. Res., Vol. 2, No. 1, 2015, pp. 60-71.
[5] N. Jalbani, M. Soylak, “Ligandless ultrasonic-assisted and ionic liquid-based dispersive liquid-liquid microextraction of copper, nickel and lead in different food samples,” Food Chem., 167, 2015, pp.433-437.
[6] F. Tadayon, M. Hanasaei, M. Madadi, “Determination and preconcentration of manganese using ionic liquid based microextraction technique in biological samples,” Academic Research International., Vol. 4, 2013, No. 4.
[7] S. Z. Mohammadi, Y. M. Baghelani, and F. Mansor, “Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination,” Quim. Nova., Vol.35, 2012, pp.198-202.
[8] J. L. Manzoori, and G. Karim-Nezhad, “Development of a cloud point extraction and preconcentration method for cd and ni prior to flame atomic absorption spectrometric determination,” Anal. Chim. Acta., 521, 2004, pp. 173-177.
[9] N. Jalbani, M. Soylak, “ Ligandless ultrasonic-assisted and ionic liquid-based dispersive liquid-liquid microextraction of copper, nickel and lead in different food samples,” Food Chem., 167, 2015, pp.433-437.
[10] Molaakbari et al., “Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination,” Journal of Hazardous Materials., 185, 2011, pp.647-652.
[11] Li. Et al., “Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples,” Spec. Chim. Acta. PartB., 64, 2009, pp. 666-671.
[12] M. Vaezzadeh, F. Shemirani, B. Majidi., “Microextraction technique based on ionic liquid for preconcentration and determination of palladium in food additive, sea water, tea and biological samples,” Food and Chem Toxicology., 48, 2010, pp. 1455-1460.
[13] A. Tadayon, R. Jamshidi, A. Esmaeili., “Delivery of tissue plasminogen activator and streptokinase magnetic nanoparticles to target vascular diseases,” Inter. J. Pharmaceutics., 495, 2015, pp. 428-438.
[14] M. Madani-Tonekaboni, M. Kamankesh, A. Mohammadi., “Determination of furfural and hydroxymethyl furfural from baby formula using dispersive liquid-liquid microextraction coupled with high performance liquid chromatography and method optimization by response surface methodology,” Journal of Food Composition and Analysis., 2015.