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.     

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.     

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.     

Preconcentration of trace levels of cadmium (ІІ) ion using <Emphasis Type="Italic">Descurainia Sophia</Emphasis> seeds as a green adsorbent for solid phase extraction followed by its determination by flame atomic absorption spectrometry

For the first time, Descurainia Sophia (DS) seeds as an efficient and green adsorbent were used in solid phase extraction for preconcentration of trace levels of cadmium prior to its determination by flame atomic absorption spectrometry (FAAS). By using a batch method, Descurainia Sophia seeds were used as adsorbent to retain cadmium (??) ions in the sample solution. After eluting the adsorbent with 3 mol L^?1 HCl, the retained cadmium (??) was determined by flame atomic absorption spectrometry. Different parameters affecting the extraction efficiency such as pH, amounts of adsorbent, type and concentration of eluent solvent, extraction and desorption time were investigated and optimized. Under the optimum conditions, the calibration curve was linear in the range of 5–300 µg L^?1 cadmium (??) with a correlation coefficient of 0.998. The limit of detection (LOD) was 1.0 µg L^?1 and the relative standard deviation (RSD, %) based on seven replicate analysis of 25 µg L^?1 cadmium (??) was 3.2%. The accuracy of the proposed method was checked by the analysis of certified reference material (CRM) and spike methods. The results show a good agreement with certified values. The proposed method was successfully applied to determination of trace levels of cadmium in different water and rice flour samples.     

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.     

Application of beech sawdust for removal of heavy metals from water: biosorption and desorption studies

In this work the efficiency of applying non-modified beech sawdust for the removal of Cu²⁺ and Cr³⁺ heavy metal ions from water solutions was examined. Parameters taken into consideration in the analysis of environment conditions were influence of sorbent concentration, initial concentration of metal ions, temperature effect, presence of additional substances in solution (NaCl and MgCl₂ inorganic salts and anionic and cationic surface-active compounds). Results of kinetic experiments were described by two models: pseudo-first-order and pseudo-second-order; equilibrium results were approximated with five non-linear isotherm models. Maximum sorption capacity at a temperature of 20 °C and pH 5.0 was 30.22 mg g^?1 for Cu²⁺ ions and 41.86 mg g^?1 for Cr³⁺ ions. The positive value of the thermodynamic parameter ΔH° indicates the endothermic nature of the process. Application of 0.1 M HCl as the eluent enables effective desorption of precious metals and reuse of sorbent for purifying water solutions of Cu²⁺ and Cr³⁺ ions.     

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.     

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.     

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 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.     

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.     

Determination of Sulfonamides in Chicken Meat by Magnetic Molecularly Imprinted Polymer Coupled to HPLC-UV

In this work, Fe₃O₄ magnetic nanoparticles were synthesized and modified by a molecularly imprinted polymer for easy and selective extraction and determination of sulfonamides in chicken meat samples. Imprinted polymer magnetic nanoparticles were characterized by Fourier transform infrared spectroscopy, X-ray diffraction pattern, thermal analysis, and scanning electron microscope micrograph. The template was removed by methanol elution. The effective parameters on extraction and determination of sulfonamides on the sorbent such as eluent type, extraction solvent, and adsorption and desorption times were optimized. Sulfonamide separation and determination were performed by high-performance liquid chromatography–UV. The linear ranges for sulfonamides were 0.5–150 μg/L and the limits of detection were 0.1–0.5 μg/L. Relative standard deviations were within 4.3–5.4 %. The method showed good selectivity for extraction of sulfonamides in real samples.     

A novel 4-(2-pyridylazo) resorcinol functionalised magnetic nanosorbent for selective extraction of Cu(II) and Pb(II) ions from food and water samples

This paper describes a novel sorbent based on 4-(2-pyridylazo) resorcinol functionalised magnetic nanoparticles and its application for the extraction and pre-concentration of trace amounts of Cu(II) and Pb(II) ions. The nanosorbent was characterised by Fourier transform infrared spectroscopy, X-ray powder diffraction, thermal analysis, elemental analysis and scanning electron microscopy. The effects of various parameters such as pH, sorption time, sorbent dosage, elution time, volume and concentration of eluent were investigated. Following the sorption and elution of analytes, Cu(II) and Pb(II) ions were quantified by flame atomic absorption spectrometry. The limits of detection were 0.07 and 0.7 μg l^?1 for Cu(II) and Pb(II), respectively. The relative standard deviations of the method were less than 7%. The sorption capacity of this new sorbent were 92 and 78 mg g^?1 for Cu(II) and Pb(II), respectively. Finally this nanosorbent was applied to the rapid extraction of trace quantities of Cu(II) and Pb(II) ions in different real samples and satisfactory results were obtained.     

Optimization of Matrix Solid-Phase Dispersion Method for Extraction of Aflatoxins from Cornmeal

An extraction method for simultaneous determination of aflatoxins (AFLAs) G2, G1, B2, and B1 in cornmeal, based on vortex-assisted matrix solid-phase dispersion (MSPD) and high-performance liquid chromatography (HPLC) with fluorescence detection was optimized by a central composite design, validated and applied. Multivariate analysis was performed to evaluate the effect of cornmeal composition on AFLA extraction. The amount and proportion of solid support (celite and C18) and volume of elution solvent (methanol and acetonitrile) were the variables tested. The mobile phase of methanol/acetonitrile/water (24:14:62, v/v/v) in isocratic elution mode provided satisfactory AFLA separation. The best recoveries (85.7 to 114.8%) were obtained when the sample preparation contained 25 mg C18 as solid support and 10 mL of elution solvent. The limits of detection ranged from 0.01 to 0.04 ng g^?1, and the limits of quantification varied from 0.02 to 0.1 ng g^?1. The optimized method was suitable for coarse and medium grind cornmeal. Multivariate correlation analysis showed that the main interferers for AFLA recovery were proteins and sugars.     

Hybrid Amine-Functionalized Titania/Silica Nanoparticles for Solid-Phase Extraction of Lead,Copper, and Zinc from Food and Water Samples: Kinetics and Equilibrium Studies

In the present study, hybrid amine-functionalized titania/silica nanoparticles were employed as a new and novel adsorbent for solid-phase extraction of Pb²⁺, Cu²⁺, and Zn²⁺ ions prior to their determination using flame atomic absorption spectrometry. Under the best conditions (including adsorbent, 0.4 g; eluent, 5.0 mL nitric acid (HNO₃), 3.0 mol L^?1, 1.0 mL min^?1; and sample, pH 5.0, 3.0 mL min^?1), detection limits, adsorption capacities, and preconcentration factors were 0.12–0.24 μg L^?1, 7.1–20.7 mg g^?1, and 200, respectively. To predict the adsorption isotherms, different isotherm models were studied and the obtained results showed that the Langmuir model is the most suitable one to explain the experimental data. The kinetics of the reaction followed pseudo-second-order kinetic model. Thermodynamic parameters like free energy (ΔG ⁰) and enthalpy (ΔH ⁰) confirmed the spontaneous and exothermic nature of the process. The method was successfully applied for determination of the analytes in different food and water samples.     

Rapid Determination of Trace Sulfonamides in Milk by Graphene Oxide-Based Magnetic Solid Phase Extraction Coupled with HPLC–MS/MS

A simple and rapid method based on magnetic solid-phase extraction (MSPE) combined with high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC–MS/MS) was used for the determination of 15 sulfonamides from milk samples. The extraction and cleanup used a graphene oxide-based magnetic nanocomposite (Fe₃O₄@GO) as an adsorbent. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe₃O₄@GO, the extraction time, the ionic strength of sample solution, and the type of eluent, were investigated. Under optimized experimental conditions, good linearity was observed in the range of 2.0 to 100.0 μg L^?1 for all of the analytes, with correlation coefficients (R²) ranging from 0.994 to 0.999. The limits of detection for the method ranged between 0.02 and 0.13 μg L^?1. Mean values of the relative standard deviation of intraday and interday precision ranging from 1.0 to 7.3 % and from 1.7 to 8.1 % were obtained, respectively. The average recoveries were between 73.4 and 97.4 % at three different spiked levels. It was confirmed that the Fe₃O₄@GO nanocomposite was an effective MSPE material for use in sulfonamide analyses in milk samples.     

Optimized Dispersive Liquid–Liquid Microextraction and Determination of Sorbic Acid and Benzoic Acid in Beverage Samples by Gas Chromatography

A new rapid method for direct determination of trace levels of sorbic and benzoic acids was developed by dispersive liquid–liquid microextraction and gas chromatography with flame ionization detection. In the proposed approach, the separation procedure of sorbic and benzoic acids was performed on a general chromatographic column without any prior derivatization processes. Some effective parameters on the microextraction recovery were studied and optimized utilizing multilevel factorial and central composite experimental designs. The best concurrent extraction efficiency acquired using ethanol and chloroform as dispersive and extraction solvents. Central composite design (CCD) resulted in the optimized values of microextraction parameters as follows: 1.0 mL of dispersive and 0.1 mL of extraction solvents, ionic salt concentration of 50 g?L^?1 at pH 4. Under optimum conditions, the calibration curve was linear over the range 0.5–20 mg L^?1. Relative standard deviation was 11% and 13% for five repeated determinations for sorbic and benzoic acids, respectively. Limits of detection were acquired as 0.2 mg L^?1 for sorbic acid and 0.5 mg L^?1 for benzoic acid. The average recoveries were 31% and 39% for sorbic and benzoic acids, respectively. The method was successfully applied to the determination of sorbic and benzoic acids as preservatives in beverage samples.     

Determination of Trans-resveratrol in Wines,Spirits, and Grape Juices Using Solid-Phase Micro Extraction Coupled to Liquid Chromatography with UV Diode-Array Detection

Solid phase microextraction (polyacrylate fiber), coupled to liquid chromatography with UV diode-array detection, has been optimized for the determination of trans-resveratrol in wines, spirits, and grape juices. The main aspects influencing fiber adsorption (fiber coating, extraction time, ethanol content, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition, carryover) of the analyte have been investigated. The method permitted a fast and simple determination of free trans-resveratrol in commercial samples. It was found in all the analyzed samples at concentration levels ranging from 0.007 to 4.486 μg mL^?1. Total trans-resveratrol concentrations were also evaluated after enzymatic deconjugation of piceid.     

Determination of Free Amino Acids in Coated Foods by GC–MS: Optimization of the Extraction Procedure by Using Statistical Design

The development and validation of an extraction procedure for quantification of free amino acids in coated products by MTBSTFA derivatization and GC–MS detection is described. The extraction method entailed the sample homogenization with hydrochloric acid (HCl) by stirring at 40 °C followed by two centrifugation steps. The optimum combination of the extraction variables was achieved by response surface methodology. HCl concentration and volume and stirring time influenced free amino acid extraction yield. The selected optimal extraction conditions were 5 g of sample mixed to 7.5 ml of 0.1 N HCl and stirred during 90 min. Consistency between predicted and experimental values as well as in the quality parameters was observed. The calibration curves were linear within the range 5–100 μg ml^?1 with correlation coefficient values (R ² ) higher than 0.99. Detection and quantification limits of the analytical procedure ranged from 2.10^?5 to 18.10^?2 μg μl^?1 and from 8.10^?5 to 60.10^?2 μg μl^?1, respectively. Precision was 0.20–12.59 % for run-to-run and 3.38–17.60 % for day-to-day. The accuracy is between 82.99 and 115.77 %. Nineteen amino acids were analyzed in frozen-thawed and deep-fried coated products from different origin, with cysteine being the most relevant.     

Chemometrics-Enhanced Micelle-Mediated Extraction Spectrophotometric Method for Simultaneous Determination of Cu<Superscript>2+</Superscript> and Zn<Superscript>2+</Superscript> in Medicinal Plant,Rice and Water Samples Using Continuous Wavelet Transform

A new micelle-mediated extraction method for the pre-concentration of trace amounts of Cu²⁺ and Zn²⁺ as a prior step to their simultaneous spectrophotometric determination has been developed in various samples. The analytes were complexed with new synthesized ligand 4,4′-((4-chlorophenyl)methylene)bis(1,3-diphenyl-1H-pyrazol-5-ol) (CPBMPY) and Triton X-100 was added as a extraction agent. The optimal reaction and extraction conditions were optimized and the analytical characteristics of the method were obtained. The detection limit of the method was 0.90 and 0.30 ng mL^?1 for Cu²⁺ and Zn²⁺, respectively. Continuous wavelet transformation (CWT) of visible spectra as a very simple and accurate method was developed for the simultaneous determination of binary mixtures of Cu²⁺ and Zn²⁺ ions. A zero-crossing technique was applied on the transformed signals and the constructed calibrations were tested by analyzing the composition of the different binary mixtures. The proposed procedure successfully was applied to analysis of water, rice, and medicinal plant and reference material samples. The amounts of metal ions obtained by the proposed methods were in good agreement with those obtained by Graphite furnace atomic absorption spectrometry.