Fatma Turak

Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue) and two sweeteners (Acesulfame-K and Aspartame) in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS), is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K) and third-derivative curve (for Aspartame) and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS), depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1 and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%); recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.

Sumac Leaves as a Novel Low-Cost Adsorbent for Removal of Basic Dye from Aqueous Solution

Sumac Leaves (SL) (Rhus Coriaria L. ) were investigated as an inexpensive and effective adsorbent for the adsorption of methylene blue (MB) from aqueous solution. The effects of initial dye concentration, initial solution pH, phases contact time, and adsorbent dose on the adsorption of MB on SL were investigated. The amount of dye adsorbed was found to vary with initial solution pH, Sumac Leaves dose, MB concentration, and phases contact time. The Langmuir and Freundlich adsorption models were evaluated using the experimental data and the experimental results showed that the Langmuir model fits better than the Freundlich model. The maximum adsorption capacity was found to be 151.69 mg/g from the Langmuir isotherm model at 25°C. The value of the monolayer saturation capacity of SL was comparable to the adsorption capacities of some other adsorbent materials for MB. The adsorption rate data were analyzed according to the pseudo-first order kinetic and pseudo-second order kinetic models and intraparticle diffusion model. It was found that kinetic followed a pseudo-second order model.

Four Derivative Spectrophotometric Methods for the Simultaneous Determination of Carmoisine and Ponceau 4R in Drinks and Comparison with High Performance Liquid Chromatography

Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130).

Arsenic speciation in water and biota samples at trace levels by ion chromatography inductively coupled plasma-mass spectrometry

ABSTRACT A sensitive, reliable, simple and rapid analytical method was developed for the determination of arsenite [As(III)], arsenate [As(V)] and arsenobetaine (AsB) species using ion chromatography combined with inductively coupled plasma-mass spectrometry (IC-ICP-MS). Inorganic and organic arsenic species were separated with an anion exchange column (Dionex AS9) and a 50 mM sodium bicarbonate mobile phase (pH 10) at a flow rate of 1.0 mL min−1. %RSD values were found to be lower than 5.1% for all arsenic species. The limits of detection (LOD) obtained for As(III), As(V) and AsB were 16.5 ng L−1, 14.1 ng L−1 and 6.2 ng L−1, respectively. The developed analytical method was tested using AsB certified reference material (NMIJ CRM 7901-a), and spring water certified reference material (UME CRM 1201) for accuracy check. This method was applied for the quantitative determination of arsenic species in different water samples and chicken samples as a solid matrix.

Accurate determination of pesticides, hormones and endocrine disruptor compounds in complex environmental samples using matrix dilution and matrix matching with dispersive liquid–liquid microextraction

Abstract Quantitative determination of contaminants in environmental samples is usually hampered by low analyte recovery which results from the complex nature of the sample matrix. This study presents the application of a developed dispersive liquid–liquid microextraction method for the determination of 12 analytes in environmental samples including sea water, fresh water (lake, well and tap water), brackish water and soil samples. Matrix matched standards were used to compensate for the low analyte recovery recorded by the conventional calibration method. The effect of matrix dilution on analyte recovery was also tested. All matrix matched and matrix diluted spiked recoveries were done concurrently with calibration standards prepared in deionized water. Percent recoveries recorded for the analytes according to deionized water calibration standards ranged between 66 and 137%. Matrix matching and matrix dilution yielded close to 100% recovery results, but the later lowered the detection limit according to the dilution factor.

Development of a sensitive closed batch vessel hydride generation atomic absorption spectrometry method for the determination of cadmium in aqueous samples

ABSTRACT Hydride generation atomic absorption spectrometry was used as a simple, sensitive, and economical method for the determination of cadmium at trace levels. This study includes a stepwise optimization of all parameters that have an impact on the production, transport, and atomization of cadmium hydride for rapid determination due to the unstable nature of the hydride produced. The cell temperature for atomization, pump period, and flow rate of carrier gas were varied, and the best conditions were defined to obtain lower detection limits. In addition, the acid and sodium borohydride concentrations were optimized since they directly affect the production of the cadmium hydride. Under optimum experimental conditions, the hydride generation efficiency was greatly enhanced to record optimized analytical signals. The accuracy of the method was determined by the analysis of a certified reference material, and the results were in good agreement with the certified value. A linear dynamic range for cadmium was observed from 0.10 to 2.0 µg/L. High sensitivity was obtained with a limit of detection of 0.029 µg/L.

Simultaneous Determination of Chromium Species in Water and Plant Samples at Trace Levels by Ion Chromatography–Inductively Coupled Plasma-Mass Spectrometry

Abstract Ion chromatography–inductively coupled plasma-mass spectrometry (IC–ICP-MS) was used for the identification and quantification of chromium species. Chromium(III) and chromium(VI) were separated and determined by IC–ICP-MS. The separation was achieved using an anion exchange column with 0.55 M HNO3 as mobile phase. It was a particular goal of this work to exclusively use nitric acid for elution in order to reduce interferences in the ICP-MS system. Analytical figures of merit were calculated under the optimum conditions by developing calibration plots in a concentration range of 0.50–250 µg/L for both species. The detection limits for Cr(III) and Cr(VI) were 0.09 and 0.03 µg/L, respectively. Spiked recovery tests were used to evaluate the applicability of the analytical method in environmental samples, and the recoveries ranged between 97 and 103% for both analytes. The accuracy of the method for total chromium content was validated through the analysis of a spring water-certified reference material (UME 1201), and the obtained results were in good agreement with the certified value. Lettuce seedlings were cultivated to evaluate the intake levels of these species. In addition, the bioaccessibility of Cr(III) and Cr(VI) from the lettuce seedlings in simulated gastric and intestinal fluids media was examined.

Sorption of Zn(II) and Pb(II) Ions by a New Resin Synthesized from Sumac Tannin and Gelatin

Recently, the interest on biomaterials and especially in tannins was growing and some attractive results were obtained in the adsorption of some metals by tannin adsorbents. Tannins are widely distributed in nature and have multiple adjacent polyhydroxyphenyl groups in their chemical structure which have extremely high affinity for heavy metal ions. This study will describe how tannin can be used as an effective zinc and lead sorbent by the use of tannin resins. Batch method was used in the experiments in which pH profile, adsorption time, adsorbent/liquid ratios, initial concentration of metal ions, adsorbent amount and temperature were investigated to determine binding properties of adsorbent for the Zn(II) and Pb(II) ions.

Sorption of Pb(II) and Zn(II) Ions from Aqueous Solution by Tannin Resins

Recently, the interest on biomaterials and especially in tannins was growing and some attractive results were obtained in the adsorption of some metals by tannin adsorbents. Tannins are widely distributed in nature and have multiple adjacent poly- hydroxyphenyl groups in their chemical structure which have extremely high affinity for heavy metal ions. This study will describe how tannin can be used as an effective zinc and lead sorbent by the use of tannin resins. Batch method was used in the experiments in which pH profile, adsorption time, adsorbent/liquid ratios, initial concentration of metal ions, adsorbent amount and temperature were investigated to determine binding properties of adsorbent for the Zn(II) and Pb(II) ions.

Simultaneous Spectrophotometric Determination of Food Additives (Benzoic Acid, Caffeine, Aspartame and Acesulfame-K) in Cola Drinks by PLS Multivariate Calibration Method

Aspartame (Apt), Acesulfame-K (Ace-K) low-calorie, high-potency artificial sweeteners are currently used in beverages and dietary food and drinks. Their increased application in food and drink products has given a new impetus to develop fast and accurate methods for their determination. Absorption spectra of Asp, Caf, Ace-K and BA strongly overlap. Therefore a direct determination of these analytes in quaternary mixture is impossible without a separation step. In order to overcome this difficulty partial least squares (PLS) method has been proposed. A spectrophotometric method for the routine, rapid end simultaneous determination of Ace-K, Caf, Aspt and BA in cola drinks was investigated. A calibration set contain- ing between 3 - 5 μ g mL -1 of Ace-K, Caf, and BA, 5 - 7 μ g mL -1 of Aspt was used. The method involves the use of 27 standard mixtures of the four compounds assayed, considered at three concentration levels and measured of samples in a 0.1 N H 3 PO 4 . The designed and optimized training set of calibration was applied to the determination of four food additives in several synthetic mixtures. Three com- mercial cola drinks (coca-cola, pepsi-cola, cola-turka) that contained the four addi- tives were also satisfactorily analyzed without separation step.