Determination of Trace Amounts of Cd(II), Cu(II), and Ni(II) in Food Samples Using a Novel Functionalized Magnetic Nanosorbent

This work describes a novel sorbent based on functionalization of magnetic nanoparticles by 2-aminobenzothiazole and its application in the extraction and preconcentration of trace amount of Cd(II), Cu(II), and Ni(II) ions. This nanosorbent was characterized by Fourier transfer infrared spectroscopy, thermal analysis, X-ray powder diffraction, elemental analysis, and scanning electron microscopy. The effects of various factors such as pH value, sorption time, sorbent dosage, type, volume, and concentration of the eluent as well as the elution time were investigated. Following the sorption and the elution of target analytes, the Cd(II), Cu(II), and Ni(II) ions were determined by flame atomic absorption spectrometry. Under the optimal conditions, the limits of detection (LODs) were 0.03, 0.009, and 0.1 μg L^?1 for Cd(II), Cu(II), and Ni(II), respectively. Linearity was within the range of 0.1–75 ng mL^?1 for Cd(II), 0.03–50 ng mL^?1 for Cu(II), and 0.5–100 ng mL^?1 for Ni(II) in the initial solution with r ² values greater than 0.9978. The relative standard deviations of the method were less than 8.4 %. The preconcentration factor of the method was 277. The sorption capacity of this new sorbent was 65, 78, and 49 mg g^?1 for Cd(II), Cu(II), and Ni(II), respectively. The proposed method was validated using two certified reference materials (LGC 6010 hard drinking water and NIST SRM 1515 apple leaves) in order to exhibit its applicability. Ultimately, this method was applied to the rapid extraction of the trace quantities of Cd(II), Cu(II), and Ni(II) ions in different food samples, and satisfactory results were obtained.     

A Nanocomposite Based on Dipyridylamine Functionalized Magnetic Multiwalled Carbon Nanotubes for Separation and Preconcentration of Toxic Elements in Black Tea Leaves and Drinking Water

A novel functionalized magnetic multiwalled carbon nanotube composite was prepared and utilized as a nanosorbent for separation and preconcentration of Cr(III), Cd(II), Cu(II), Pb(II), and Ni(II) ions. The synthesized nanosorbent was characterized with various techniques. The parameters influencing the preconcentration efficiency were optimized through experimental design methodology by using Box-Behnken design method. Uptake time, pH of sample, and magnetic nanosorbent amount were evaluated in the sorption step as the main affecting factors, while four variables including type, volume, concentration of the eluent, and elution time were considered in the elution step. After sorption and elution steps, the target analytes were determined by flame atomic absorption spectrometry. Limit of detection was 0.5, 0.08, 0.7, 0.4, and 0.1 ng mL^?1 for Cr(III), Cu(II), Pb(II), Ni(II), and Cd(II) ions, respectively. All relative standard deviations of the method were <9.5%. The capacity of the sorbent ranged between 184 and 215 mg g^?1. Finally, the developed method was successfully applied to the rapid extraction of trace amounts of these ions from black tea leaf samples and drinking water.     

Synthesis,characterisation and analytical application of Fe3O4@SiO2@polyaminoquinoline magnetic nanocomposite for the extraction and pre-concentration of Cd(II) and Pb(II) in food samples

This work describes a novel Fe₃O₄@SiO₂@polyaminoquinoline magnetic nanocomposite and its application in the pre-concentration of Cd(II) and Pb(II) ions. The parameters affecting the pre-concentration procedure were optimised by a Box–Behnken design through response surface methodology. Three variables (extraction time, magnetic sorbent amount and pH) were selected as the main factors affecting the sorption step, while four variables (type, volume and concentration of the eluent, and elution time) were selected as main factors in the optimisation study of the elution step. Following the sorption and elution of analytes, the ions were quantified by flame atomic absorption spectrometry (FASS). The limits of detection were 0.1 and 0.7 ng ml^?1 for Cd(II) and Pb(II) ions, respectively. All the relative standard deviations were less than 7.6%. The sorption capacities of this new sorbent were 57 mg g^?1 for Cd(II) and 73 mg g^?1 for Pb(II). Ultimately, this nanocomposite was successfully applied to the rapid extraction of trace quantities of these heavy metal ions from seafood and agricultural samples and satisfactory results were obtained.     

Determination of heavy metal ions in vegetable samples using a magnetic metal–organic framework nanocomposite sorbent

This paper describes the synthesis and application of a novel magnetic metal–organic framework (MOF) [(Fe₃O₄-benzoyl isothiocyanate)/Cu₃(benzene-1,3,5-tricarboxylate)₂] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box–Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l^–1 EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml^?1 for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l^?1 of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe₃O₄-benzoyl isothiocyanate)/MOF] was 175 mg g^?1 for Cd(II), 168 mg g^?1 for Pb(II), 210 mg g^?1 for Zn(II) and 196 mg g^?1 for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe₃O₄-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.     

Application of Polypropylene Amine Dendrimers (POPAM)-Grafted MWCNTs Hybrid Materials as a New Sorbent for Solid-Phase Extraction and Trace Determination of Gold(III) and Palladium(II) in Food and Environmental Samples

A new method which utilizes a polypropylene amine dendrimers (POPAM)-grafted multi-walled carbon nanotubes (MWCNTs) hybrid materials as an effective sorbent in solid-phase extraction has been developed for separation and preconcentration of Au(III) and Pd(II) trace levels in food, water and soil samples. The optimum experimental conditions such as pH, flow rates, type, concentration, and volume of the eluent for elution of gold and palladium ions, breakthrough volume, and effect of potentially interfering ions on separation and determination of these noble metals were investigated. The extraction recoveries for the mentioned noble metals were greater than 98 % and the limits of detection were 0.08 and 0.12 ng mL^?1 for gold and palladium, respectively. The relative standard deviations of the method were less than 4 % for eight separate column experiments for determination of 5.0 μg of gold and palladium ions. The adsorption capacity of the modified MWCNT was 92 mg g^?1 for gold and 74 mg g^?1 for palladium on POPAM-grafted MWCNTs. Validation of the suggested method was performed by analyzing certified reference materials. Finally, the proposed method was applied for determination of gold(III) and palladium(II) in real samples, including fish, shrimp, water, and soil.     

Determination of Pb(II) Ions Using Novel Ion-Imprinted Polymer Magnetic Nanoparticles: Investigation of the Relation Between Pb(II) Ions in Cow’s Milk and Their Nutrition

The application of novel Pb(II) ion-imprinted polymer coated on magnetic mesoporous silica was investigated in preconcentration and determination of low level of Pb(II) ions. The job proposed a new method for preconcentration and determination of Pb(II) ions. This novel sorbent was characterized by scanning electron microscopy, thermal gravimetric/differential thermal analysis, elemental analysis, and low-angle X-ray powder diffraction. Effects of various factors such as the effects of the pH of sample solution, eluent (include type, concentration and volume), adsorption and desorption time which are effective in method efficiency, were appraised through this study. In order to investigate the selectivity of this sorbent toward Pb(II) ion, the effects of variety of foreign ions interfering on preconcentration and recovery of Pb(II) ions were also investigated. The limit of detection (LOD) was found to be 0.7 μg L^?1 and the recovery and relative standard deviation of the method were 96.6–102.4 % and 1.3–3.3 %, respectively. Validation of the outlined method was performed by analyzing several standard reference materials with certified Pb(II) concentrations. Finally, this sorbent was applied for separation and determination of Pb(II) ion in grass and cow’s milk, which showed their lead concentration to be below the detection limit of flame atomic adsorption spectroscopy.     

Graphene-Based Preconcentration System Prior to Energy Dispersive X-Ray Fluorescence Spectrometric Determination of Co,Ni, and Cu Ions in Wine Samples

A combination of dispersive micro solid-phase extraction (DMSPE), based on graphene as a solid sorbent, with energy dispersive X-ray fluorescence spectrometry (EDXRF) is proposed for preconcentration and determination of Co(II), Ni(II), and Cu(II) ions in wine samples. In the developed procedure, cupferron complexes of metal ions are adsorbed on graphene dispersed in aqueous samples. After the adsorption process, aqueous samples are passed through a membrane filter with the use of filtration assembly, and then loaded filters are directly measured using EDXRF. In order to obtain high recovery of the metal ions, various analytical parameters influencing sorption were optimized, such as pH, amount of graphene, Triton X-100 and cupferron, sample volume, and sorption time. Under optimal conditions, the calibration plots cover the 2 to 100 ng mL^?1 range for Co(II) and Ni(II), and 2 to 150 ng mL^?1 for Cu(II). The detection limits of 0.08, 0.08, and 0.07 ng mL^?1 for Co(II), Ni(II), and Cu(II) were obtained using 50 mL sample volume and 200 μg of graphene. The precision (at a 20 ng mL^?1 level for n?=?10) is lower than 3.5 %. The proposed method was successfully applied to determination of Co, Ni, and Cu in wine samples.     

Application of a New Functionalized Nanoporous Silica for Simultaneous Trace Separation and Determination of Cd(II), Cu(II), Ni(II), and Pb(II) in Food and Agricultural Products

A novel sorbent for simultaneous separation of cadmium, copper, nickel, and lead was prepared by functionalizing SBA-15 nanoporous silica with dithizone. A solid-phase extraction method using the above sorbent was developed to separate and preconcentrate trace amounts of cadmium, copper, nickel, and lead ions from food and agricultural products by flame atomic absorption spectrometry measurements. The optimum experimental conditions such as pH; flow rates; type, concentration, and volume of the eluent; breakthrough volume; and effect of coexisting ions on the separation and determination of these heavy metals were evaluated. The extraction efficiencies for the mentioned heavy metals were greater than 97 %, and the limits of detection were 0.09, 0.16, 0.21, and 0.45 μg?L^?1 for cadmium, copper, nickel, and lead, respectively. The preconcentration factor for simultaneous analysis of the four heavy metals was found to be 100 approximately. The relative standard deviations of the method were <5 % for 10 separate column experiments for the determination of 5.0 μg of cadmium, copper, nickel, and lead ions. The adsorption capacity of the dithizone-SBA-15 was 189 mg?g^?1 for cadmium, 102 mg?g^?1 for copper, 91 mg?g^?1 for nickel, and 208 mg?g^?1 for lead.     

Monitoring of Zn(II), Cd(II), Pb(II) and Cu(II) During Refining of Some Vegetable Oils Using Differential Pulse Anodic Stripping Voltammetry

In this study, a novel approach has been developed using differential pulse anodic stripping voltammetry (DPASV) for the simultaneous determination of Zn(II), Cd(II), Pb(II) and Cu(II) in edible oils at hanging mercury drop electrode. The microwave digestion of oil samples was carried out with concentrated HNO₃ and H₂O₂. KNO₃ was used as a supporting electrolyte. The experimental conditions optimized such as deposition time, stirring rate and size of mercury drop were 300 s, 600 rpm and 10 mm², respectively. The method was applied to quantify Zn(II), Cd(II), Pb(II) and Cu(II) in crude and refined hazelnut, corn, sunflower and olive oils. During refining of different vegetable oils, the removal efficiencies of Zn(II), Cd(II), Pb(II) and Cu(II) were calculated as 98.20–99.91, 98.50–99.90, 95.26–99.76 and 95.93–99.92 %, respectively. The limits of detection for Zn(II), Cd(II), Pb(II) and Cu(II) were 2.1?×?10^?8, 8.7?×?10^?10, 7.1?×?10^?9 and 3.4?×?10^?9 and the limits of quantification were 6.8?×?10^?8, 2.9?×?10^?9, 2.3?×?10^?8 and 1.1?×?10^?8 M with linear regression coefficients (R ²) of 0.9930, 0.9928, 0.9893 and 0.9931, respectively. It was observed that the above metals in crude and refined vegetable oils could be determined simultaneously by the DPASV method.     

Solid Phase Extraction of Pb(II) and Cd(II) in Food,Soil, and Water Samples Based on 1-(2-Pyridylazo)-2-Naphthol-Functionalized Organic–Inorganic Mesoporous Material with the aid of Experimental Design Methodology

An effective sorbent of 1-(2-Pyridylazo)-2-naphthol-functionalized mesoporous silica has been prepared to simultaneous separation and preconcentration of lead and cadmium ions in aqueous solution. Structural characterization of 1-(2-Pyridylazo)-2-naphthol-functionalized organic–inorganic hybrid mesoporous materials was conducted by Fourier transform infrared spectroscopy, transmission electron microscopy, N₂ adsorption–desorption measurement, X-ray diffraction, and elemental and thermal analysis, which confirmed the successful grafting of organic moiety on mesoporous silica. The affecting parameters on adsorption and desorption steps were optimized by Box-Behnken design through response surface methodology. Three variables (pH value, sorption time, and amount of the sorbent) were selected as the main factors affecting sorption step, while four variables (type of eluent, eluent volume, eluent concentration, and elution time) were selected for desorption step in the optimization study. The optimized values by this optimization method were 10 mg, 8 min, 6.3, HCl, 1.6 mL, 1.2 mol L^?l HCl, and 10 min, for amount of sorbent, sorption time, pH of solution, type, volume, and concentration of the eluent, and elution time, respectively. Under the optimized conditions, the detection limits of the proposed method for lead and cadmium ions were found to be 0.9 and 0.04 μg L^?1, respectively, while the relative standard deviation (RSD) for five replicate measurements was calculated to be <3 % for both ions. For proving that the proposed method is reliable, a wide range of food, soil, and water samples with different and complex matrixes was used.     

One-Step Synthesis of Zirconia and Magnetite Nanocomposite Immobilized Chitosan for Micro-Solid-Phase Extraction of Organophosphorous Pesticides from Juice and Water Samples Prior to Gas Chromatography/Mass Spectroscopy

In this research, a magnetic sorbent was prepared by immobilizing zirconia and magnetite (Fe₃O₄) nanoparticles in chitosan, which is characterized and used as an effective nanosorbent in magnetic dispersive micro-solid-phase extraction (MDMSPE) of organophosphorous pesticides (OPPs) from juice and water samples prior to gas chromatography-mass detection (GC-MS). The properties and morphology of synthesized sorbent were characterized by scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR), vibrating sample magnetometry (VSM), and differential scanning calorimetric (DSC) analysis. The main experimental parameters including pH level, extraction time, sorbent mass, salt concentration, and desorption conditions were investigated and optimized to maximize extraction efficiency. Under optimized conditions, the calibration curves were obtained in the concentration range of 0.1–500 ng mL^?1 with correlation coefficients between 0.9993 and 0.9999. The limits of detection (signal-to-noise ratio (S/N) = 3) and limits of quantification (S/N = 10) of the method ranged from 0.031 to 0.034 ng mL^?1 and 0.105–0.112 ng mL^?1, respectively. The intra-day and inter-day RSDs were 2.2–5.7 and 2.5–7.5%, respectively. The method was successfully applied to the analysis of OPPs in fruit juices (apple, peach, and cherry) and water (mineral, tap, and river) real samples, with recoveries in the range of 86.0–106.0% for the spiked juice and water samples. The results showed that with combination of high selectivity of zirconia and magnetic property of magnetite as well as immobilizing ability of chitosan, the fabricated sorbent exhibited exceptional extraction ability toward the OPPs.     

Application of Ion-Imprinted Polymer Nanoparticles for Selective Trace Determination of Palladium Ions in Food and Environmental Samples with the Aid of Experimental Design Methodology

A solid phase extraction method using Pd²⁺ ion-imprinted polymer (Pd²⁺-IIP) nanoparticles combined with flame atomic absorption spectrophotometry (FAAS) was developed for the preconcentration and trace detection of palladium ions. The Pd²⁺-IIP nanoparticles were obtained by precipitation polymerization of 4-vinylpyridine (the functional monomer), ethylene glycol dimethacrylate (the cross-linker), 2,2′-azobisisobutyronitrile (the initiator), Eriochrome Cyanine R (the lead-binding ligand), and palladium ions (the template ion) in acetonitrile solution. The parameters affecting adsorption and desorption steps were optimized by a Box–Behnken design through response surface methodology. Three variables (pH value, extraction time, and amount of the synthesized IIP) were selected as the main factors affecting sorption step, while four variables (type of eluent, volume of the eluent, concentration of the eluent, and elution time) were selected for desorption step in the optimization study. The optimized values by this optimization method were 30 mg, 15 min, 6.0, HCl, 4.0 mL, 1.8 mol L^-l HCl, and 14 min, for amount of polymer, retention time, pH of solution, type, volume, concentration of the eluent, and elution time, respectively. Under the optimized conditions, the detection limit for the proposed method was found to be 0.2 μg L^?1, while the relative standard deviation (RSD) for five replicate measurements was calculated to be <3 %. Finally, the introduced solid phase extraction technique was successfully applied for extraction and determination of Pd²⁺ ions in food and environmental samples.     

The Mesoporous Porphyrinic Zirconium Metal-Organic Framework for Pipette-Tip Solid-Phase Extraction of Mercury from Fish Samples Followed by Cold Vapor Atomic Absorption Spectrometric Determination

In this study, the highly stable mesoporous porphyrinic zirconium metal-organic framework, namely PCN-222/MOF-545 (Zr-MOF), was prepared and used for pipette-tip solid-phase extraction of Hg(II). As a high-capacity sorbent, 4 mg of the Zr-MOF was placed into a conventional pipette tip and used, for the first time, for the fast extraction and preconcentration of mercury ions. For desorption, 50 μL of 10% HCl was used by 15 repeated aspirating/dispensing cycles, and Hg ions in elusion were measured by a cold vapor atomic absorption spectrometer. Affecting parameters on extraction efficiency were studied, and optimum conditions were established as amount of sorbent 2 mg, pH was adjusted to 5.0, the eluting volume was 15 μL, and extraction was performed on 1.8 mL of the sample. The optimal number of aspirating/dispensing cycles for extraction and desorption of analytes was found to be 10 and 15 cycles, respectively. The limit of detection of the method was found to be 20 ng L^?1 with a relative standard deviation of ≤3.1% (for seven replicate analyses of 20 μg L^?1 of mercury). Adsorption capacity and enrichment factor were 35.5 mg g^?1 and 120-fold, respectively. The proposed method was successfully applied for the determination of Hg(II) ions in fish samples.     

Determination of Cd (II), Cu (II), and Pb (II) in Some Foods by FAAS after Preconcentration on Modified Silica Gels with Thiourea

Abstract: This study describes preconcentration method for determination of Cd (II), Cu (II), and Pb (II) in some food samples. Silica gel was modified with thiourea and characterized by IR and C, H, N, S elemental analysis. Modified silica gel was used as a solid phase extraction for determination of Cd (II), Cu (II) and Pb (II) in tuna fish, biscuit, black tea, rice, ka?ar cheese, honey, tomato paste, and margarine samples. The analytical conditions including eluent type, pH of sample solutions, flow rates of sample and eluent solutions, etc. were optimized. The influence of the matrix ions on the involvement of the Cd (II), Cu (II), and Pb (II) were also studied. GBW 07605 tea standard reference material was used for validation of method. The method was successfully applied for the determination of Cd (II), Cu (II), and Pb (II) ions in food samples. The detection limits were in the range of 0.81 μg/L, 0.38 μg/L, and 0.57 μg/L for cadmium, copper and lead, respectively. The relative standard deviations of the procedure were below 10%. The sorption capacities were found as 92 μmol/L Cd (II), 286 μmol/L Cu (II), and 121 μmol/L Pb (II).     

Dithizone-modified graphene oxide nano-sheet as a sorbent for pre-concentration and determination of cadmium and lead ions in food

Graphene oxide nano-sheet was modified with dithizone as a novel sorbent for selective pre-concentration and determination of Cd(II) and Pb(II) in food. The sorbent was characterised by various analytical methods and the effective parameters for Cd(II) and Pb(II) adsorption were optimised during this work. The high adsorption capacity and selectivity of this sorbent makes the method capable of fast determinations of the Cd(II) and Pb(II) content in complicated matrices even at μg l^?1 levels using commonly available instrumentation. The precision of this method was < 1.9% from 10 duplicate determinations and its accuracy verified using standard reference materials. Finally, this method was applied to the determination of Cd(II) and Pb(II) ions in common food samples and satisfactory results were obtained.     

Sorption of copper (II) ions by pine sawdust

The sawdust of Calabrian pine was used as sorbent for the removal of Cu(II) ions from aqueous solution of copper sulfate pentahydrate (CuSO₄.5H₂O) at different concentrations, pHs and temperatures. The results showed that about 65–81% of Cu(II) ions in the solution could be adsorbed on the sawdust. The percentage of adsorped Cu(II) ions onto the sawdust increased with increasing initial concentration. Kinetic studies indicated that the sorption process followed the first order reversible kinetic model. It was also determined that the sorption process obeyed the Freundlich isotherm. Furthermore, the sorption thermodynamic was investigated in detail.     

Selective Determination of Selenium in Garlic, Mushroom and Water Samples by Chemically Modified Mesoporous Silica Solid Phase Coupled with ICP-OES

A selective sorbent for solid phase extraction (SPE), based on a chemically modified mesoporous silica (SBA-15), followed by inductively coupled plasma-optical emission spectrometry was used for extraction, preconcentration, and determination of selenium in water and food samples. The main parameters of SPE including pH, amount of mesoporous (solid phase), concentration of the eluent (desorption solvent), and equilibrium time were optimized by using a fractional central composite design (f-CCD). The optimum conditions were found to be 3.2 for pH, 21 mg for amount of the mesoporous, 1 mol l^?1 for eluent concentration, and 9 min for equilibrium time. Under the optimal conditions, the limit of detection (LOD) was 2.56 μg l^?1. The linear dynamic range (LDR) was 5–1,000 μg l^?1 with determination coefficient (R ²) of 0.999. Relative standard deviation (C?=?400 μg l^?1, n?=?5) was 3.84 %. The enrichment factor was 20. The maximum sorption capacity of the modified SBA-15 was 15 mg g^?1. The sorbent presented good stability, reusability, high adsorption capacity, and fast rate of equilibrium for sorption/desorption of selenium (IV) ions.     

A Preconcentration Procedure for Determination of Ultra-Trace Mercury (II) in Environmental Samples Employing Continuous-Flow Cold Vapor Atomic Absorption Spectrometry

New functionalized magnetic nanoparticles as solid-phase sorbent were prepared and investigated for extraction of ultra-trace amounts of mercury from environmental samples. The Fe₃O₄ magnetic nanoparticles functionalized with dithizone were characterized by Fourier transform infrared spectrometer. X-ray diffraction and scanning electron microscopy confirmed the size of nanoparticles. Effects of several factors on the extraction procedure were investigated. The optimized conditions were established to be 80 mg of polymer, 8.5 for solution pH, 5 min for adsorption time, 5 min for desorption time, 2 mL for HCl (0.1 mol L^?1)/ thiourea 0.05 % as the eluent, 500 mL for breakthrough volume, and without addition of salt. Under the optimal conditions, the limit of detection, maximum capacity, and preconcentration factor were 0.05 ng mL^?1, 0.557 mmol g^?1, and 250, respectively. Limit of quantification was in the range of 0.2–2 ng mL^?1 for various matrices. Accuracy and precision of the method were about ±2.0 and below 11.1 %, respectively. Finally, the present method has been successfully applied to mercury determination in table salt, green tea, vegetables, toothpaste, and water samples. The mercury content found in the real samples was from 0.6 to 15.74 ng mL^?1 without addition of mercury.     

Method for the determination of cadmium,lead, nickel,cobalt and copper in seafood after dispersive liquid–liquid micro-extraction

A method using dispersive liquid–liquid micro-extraction (DLLME) and detection by inductively coupled plasma optical emission spectroscopy (ICP-OES) was developed for the determination of trace elements in seafood samples. The procedure allowed the simultaneous determination of Cd(II), Pb(II), Ni(II) Cu(II) and Co(II) after pre-concentration using sodium diethyldithiocarbamate (DDTC) as a chelating agent. Under optimised conditions, the method had a limit of detection (LOD) of 0.03, 0.11, 0.12, 0.18 and 0.12 µg l^?1 for Cd(II), Pb(II), Ni(II) Cu(II) and Co(II), respectively. The following enrichment factors were obtained: 16 (Cd), 34 (Pb), 20 (Ni) 34 (Cu) and 12 (Co). The procedure was applied for the determination of these elements in seafood (shrimp, mussel, bass and mullet) samples. The method is simple, efficient and easy to perform for the simultaneous determination of elements in seafood samples by ICP-OES.     

Simultaneous pre-concentration of Pb and Sn in food samples and determination by atomic absorption spectrometry

A cloud point extraction (CPE) method has been developed for the pre-concentration and simultaneous determination of lead [Pb(II)] and tin [Sn(II)] using Acridine Orange as complexing reagent and mediated by nonionic surfactant (Triton X-114) by flame atomic absorption spectrometry (FAAS). The main factors affecting analytical performance of CPE have been investigated in detail. The extracted surfactant-rich phase was diluted with (1.0 mol L^?1) nitric acid in methanol, prior to subjecting FAAS. The calibration graphs obtained from Pb(II) and Sn(II) were linear in the concentration ranges of 5–1,000 and 10–5,000 μg L^?1 with detection limits of 1.40 and 2.86 μg L^?1, respectively. The relative standard deviations for 10 replicates containing 25 μg L^?1 of Pb(II) and Sn(II) were 2.15 and 2.50 %, respectively. The analytical procedure was verified by the analysis of the standard reference materials NWTMDA-61.2 (water-trace elements) and NIST SRM 1548a (typical diet). The developed method has been applied to the simultaneous determination of total Pb and Sn in canned food samples including juices, tomato paste, corn, and green pea.