A Novel Vortex Assisted Dispersive Solid Phase Extraction of Some Trace Elements in Essential Oils and Fish Oil

Feyzullah TOKAY, Refiye GÜNAYDIN, Sema BAĞDAT*

Chemistry Department, Faculty of Science and Arts, Balıkesir University, Çağış Campus, Balıkesir, 10145, Turkey
*Corresponding Author: sbagdat@balikesir.edu.tr

Abstract
In this paper, a novel vortex assisted solid phase extraction procedure combined with inductively coupled plasma optic emission spectrometry was presented for determination of Mn, Cu, Ni, Cr, Cd and Pb directly in oily matrix. The suggested separation and preconcentration method was based on simultaneous sorption of the target analytes from real essential oil matrix onto γ-Al2O3 functionalized with fluorescein (Al-Flr) and transfer to aqueous eluent prior to quantification. The effect of different parameters including sorption and elution time, sample volume, eluent type and concentration and interfering ions were investigated.  The working conditions were given as follows, vortex agitation for sorption and elution 40 s, sample volume 20 mL, eluent type HCl, eluent concentration 0.3 mol L-1. The detection limits were found to be 0.7 µg L-1 for Mn, 4.1 µg L-1 for Cu, 1.0 µg L-1 for Ni, 1.6 µg L-1 for Cr, 0.7 µg L-1 Cd and 1.0 µg L-1 Pb.  The evaluation of the accuracy and precision of the method was tested via metallo-organic certified reference material. The recovery values have warranted the accuracy and found between 98.4 – 103.3% with 2.6 – 6.4% relative standard deviation (RSD, %). The sampling frequency of the procedure was calculated as 11.25 h-1.      Finally, the proposed analytical method was successfully applied on analyte spiked and unspiked apricot, black cumin, pine turpentine, thyme, mint essential oils and fish oil samples without any need of performing mineralization pretreatments.
Keywords: essential oil, dispersive solid phase extraction, ICP OES, alumina, preconcentration

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A Novel Vortex Assisted Dispersive Solid Phase Extraction

J Am Oil Chem Soc (2010) 87:1389–1395
DOI 10.1007/s11746-010-1633-7

Copper and Iron Determination with [N,N¹-Bis(salicylidene)-2, 2^/-dimethyl-1,3-propanediaminato in Edible Oils Without Digestion

Eda Köse Baran1, Sema Bağdat Yaşar2
1Institute of Science and Technology, Balıkesir University, Çağış, 10145 Balıkesir, Turkey
2Chemistry Department, Faculty of Science and Arts, Balıkesir University, Çağış, 10145 Balıkesir, Turkey e-mail: sbyasar@balikesir.edu.tr

Received: 3 December 2009 / Revised: 4 April 2010 / Accepted: 24 April 2010 / Published online: 18 September 2010
AOCS 2010

Abstract
A new method for the determination of cop-per(II) and iron(III) in liquid edible oils which does not require a digestion step was developed. The suggested method involves extraction of metals with [N,N⁰-bis(sali-cylidene)-2,2⁰-dimethyl-1,3-propanediaminato] (LDM) followed by flame atomic absorption spectrometry mea-surement. As a first step, metal complexes of copper(II) and iron(III) ions with LDM were investigated spectro-photometrically. After the analytical properties and experimental conditions of the complexation had been determined, these findings were used to determine the extraction period as a second step. Experimental conditions were optimized using a central composite design. Optimum conditions for Cu(II) and Fe(III) extractions from oil were found: the ratios of the volume of Schiff base solution used to the mass of oil (V_LDM/m_oil; mL g^-1) were 0.76 and 1.19 mL g^-1, the stirring times were 73 and 67 min, and the temperatures were 31 and 28 LC, respectively. The developed extraction and determination method was tested on certified reference materials; the recovery percentages were found to be 99.4 ± 2.8 and 100.2 ± 5.6 for Cu(II) and Fe(III), respectively. The suggested method was per-formed on real samples such as olive oil, sunflower oil, corn oil, canola oil and recovery values between 97.2–102.1 for Cu(II) and 94.5–98.6 for Fe(III) were determined. It was concluded that the developed method has some advantages over the common traditional method including rapidity, sensitivity, accuracy, reduced risk and cost.
Keywords Edible oil Iron Copper [N,N⁰-bis (salicylidene)-2,2⁰-dimethyl-1,3-propanediaminato] Schiff base Flame atomic absorption spectrometry

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Copper and Iron Determination with

Extraction of nickel from edible oils with a complexing agent prior to determination by FAAS

Feyzullah Tokay, Sema Bağdat^*

Balıkesir University, Faculty of Science and Arts, Chemistry Department, 10145 Çağış, Balıkesir, Turkey

Abstract
In the present work, a new extraction method for separation of nickel from edible oils and determination by FAAS is reported. This method is based on extraction of Ni(II) ions from the oil to aqueous phase with N,N^/-bis(4-methoxysalicylidene) ethylenediamine (MSE) and determination by FAAS. Properties of the complex formed between MSE and Ni(II) were investigated spectrophotometrically. Central composite design (CCD) was utilized for optimization of MSE to oil, stirring time and temperature, which were 0.97 mlg^-1, 15.4 min, and 29.7 ⁰C, respectively. The developed method was tested with an oil-based metal standard and the recovery was 93.8 ± 3.9%. The proposed method was applied with five different edible oils.
Keywords: Edible oils, Nickel, N,N^/ -bis(4- ethoxysalicylidene), ethylenediamine, Schiff base, Central composite design, Flame atomic absorption spectrometry

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Extraction of nickel from edible oils