RESUMO
Despite the therapeutic properties of capsaicin for some diseases, it shows some side effects for human health. The goal of this study was to develop a precise and accurate analytical strategy for the trace determination of capsaicin in different food, biological and environmental samples including pepper, saliva and wastewater by gas chromatography-mass spectrometry (GC-MS) after spraying-based fine droplet formation-liquid phase microextraction (SFDF-LPME) and quadruple isotope dilution (ID4) method. Acetic anhydride was used as derivatizing agent, and the extraction method was used to enrich the analyte derivative to reach low detection limits. Under the optimum conditions, limit of detection (LOD) and limit of quantitation (LOQ) were determined to be 0.33 and 1.10 µg/kg, respectively. Percent recoveries calculated for SFDF-LPME-GC-MS method ranged between 84.1 and 131.7 %. After the application of ID4-SFDF-LPME-GC-MS method, percent recoveries were obtained in the range of 94.9 and 104.0 % (%RSD ≤ 2.8) for the selected samples. It is obvious that the isotope dilution-based method provided high accurate and precise results due to the elimination of errors during the derivatization, extraction and measurement steps.
Assuntos
Capsaicina , Cromatografia Gasosa-Espectrometria de Massas , Limite de Detecção , Cromatografia Gasosa-Espectrometria de Massas/métodos , Capsaicina/análise , Microextração em Fase Líquida/métodos , Humanos , Águas Residuárias/química , Saliva/química , Capsicum/química , Análise de Alimentos/métodos , Reprodutibilidade dos Testes , Anidridos Acéticos/químicaRESUMO
Garlic is in the family Liliaceae and has many different constituents such as organic sulfur compounds, amino acids, carbohydrates, minerals, and vitamins. In this work, a simple, sensitive, and accurate analytical method was developed for the determination of selected organosulfur compounds (OSCs) in garlic bulbs using reversed phase-high performance liquid chromatography (RP-HPLC). Oil-soluble and water-soluble OSCs were extracted from the garlic samples via acetonitrile and deionized water, respectively. The OSCs were separated on a Phenomenex C18 (250 mm, 4 mm, 5mm) column and the monitoring was performed with a UV detector at 220 nm. An isocratic mobile phase comprising of 0.10 M trifluoroacetic acid (TFA) in 85% acetonitrile (ACN) and 0.10 M TFA in distilled water (DW) (90: 10% v/v) was used to elute the analytes. Under optimum experimental conditions, the limits of detection (LOD) for the analytes were calculated in the range of 0.09 to 0.17 mg/kg. For the garlic sample extracts analyzed under optimal instrumental conditions, DAS (diallyl sulfide), DADS (diallyl disulfide), and DATS (diallyl trisulfide) were detected in the ranges of 8.0 to 32.5 mg/kg, 20.4 to 67.3 mg/kg, and 60.7 to 356.6 mg/kg, respectively. Spiked recovery experiments were conducted on the garlic samples to confirm the method's applicability and accuracy. The recovery results ranged between 39.0% and 90.9% for the garlic samples extracted with deionized water. The developed method is simple, precise, accurate, reliable, and time-effective for the determination of OSCs. Additionally, the green profile of the developed method was investigated by using AGREEprep software and the greenness score was recorded as 0.65, indicating that the method developed is environmentally friendly.
RESUMO
This work presents a sensitive and accurate analytical method for the determination of phenytoin at trace levels in domestic wastewater and synthetic urine samples by gas chromatography-mass spectrometry (GC-MS) after the metal sieve-linked double syringe liquid-phase microextraction (MSLDS-LPME) method. A metal sieve was produced in our laboratory in order to disperse water-immiscible extraction solvents into aqueous media. Univariate optimization studies for the selection of proper extraction solvent, extraction solvent volume, mixing cycle, and initial sample volume were carried out. Under the optimum MSLDS-LPME conditions, mass-based dynamic range, limit of quantitation (LOQ), limit of detection (LOD), and percent relative standard deviation (%RSD) for the lowest concentration in calibration plot were figured out to be 100.5-10964.2 µg kg-1, 150.6 µg kg-1, 45.2 µg kg-1, and 9.4%, respectively. Detection power was improved as 187.7-folds by the developed MSLDS-LPME-GC-MS system while enhancement in calibration sensitivity was recorded as 188.0-folds. In the final step of this study, the accuracy and applicability of the proposed system were tested by matrix matching calibration strategy. Percent recovery results for domestic wastewater and synthetic urine samples were calculated as 95.6-110.3% and 91.7-106.6%, respectively. These results proved the accuracy and applicability of the proposed preconcentration method, and the obtained analytical results showed the efficiency of the lab-made metal sieve apparatus.
Assuntos
Microextração em Fase Líquida , Poluentes Químicos da Água , Cromatografia Gasosa-Espectrometria de Massas/métodos , Águas Residuárias , Fenitoína/análise , Poluentes Químicos da Água/análise , Monitoramento Ambiental/métodos , Solventes/química , Água/análise , Microextração em Fase Líquida/métodos , Limite de DetecçãoRESUMO
This study was aimed at developing a simple and efficient CoSn(OH)6 nanocubes-based preconcentration method for the preconcentration of copper ions from cinnamon extracts for determination by flame atomic absorption spectrometry. The cube-shaped sorbent was synthesized using the simple stoichiometric co-precipitation method under ambient conditions. Experimental factors of the method were evaluated with a comprehensive optimization approach to maximize the extraction efficiency for the analyte. Under the optimal conditions, the limit of detection (LOD), limit of quantitation (LOQ), and linear dynamic range were recorded as 0.98 µg/L, 3.28 µg/L, and 4.0-75 µg/L, respectively. The enhancement factor was calculated as 101.6-fold by comparing the LODs of the optimized and direct analysis systems. Percent recoveries were found to be within an acceptable range (77.6-115 %), with high repeatability using matrix matching calibration strategy. Results validated the proposed method as a highly efficient extraction approach for the monitoring of copper ions in herbal cinnamon extracts.
Assuntos
Cinnamomum zeylanicum , Cobre , Cobre/química , Íons , Espectrofotometria Atômica/métodos , Calibragem , Concentração de Íons de Hidrogênio , Extração em Fase Sólida/métodosRESUMO
Pesticides have been used on several fruits, vegetables and cereals to control harmful organisms in order to increase the quality of products; however, these substances cause serious health effects. Therefore, an accurate and sensitive analytical method should be developed for the determination of pesticides to evaluate their toxicity. In this study, an efficient microextraction strategy was applied to preconcentrate eight different selected pesticides from mixed fruit juice samples prior to gas chromatography-mass spectrometry detection. All significant parameters such as spraying number, extraction solvent type, sample volume and mixing type/period belonging to the developed extraction method were elaborately optimized to get low detection limits. After the optimization studies, system analytical performance studies were carried out and limit of detection (LOD) values varied from 0.04 µg /kg-1 to 1.99 µg kg-1 (mass based) for the selected analytes. Under the optimum experimental conditions, spiking recovery experiments were performed in the mixed fruit juice samples to evaluate the applicability and accuracy of the proposed method. The recovery results were recorded in the range of 81.4-123.5% with acceptable standard deviations by applying a matrix matching calibration strategy. The proposed analytical method can be used for the qualitative and quantitative determination of selected pesticides in the mixed fruit juice samples and can also be applied to other fruit juice samples using a matrix matching calibration strategy.
Assuntos
Praguicidas , Praguicidas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Calibragem , Sucos de Frutas e Vegetais/análise , SolventesRESUMO
This study established the simultaneous determination of the selected endocrine-disrupting compounds (EDCs) and pesticides in rock, soil, water, moss, and feces samples collected from the Antarctic region. The spray-assisted droplet formation-based liquid phase microextraction (SADF-LPME) coupled to GC-MS system was developed and validated for the screening and monitoring of 29 selected EDCs and pesticides. Binary solvent system, 1:1 (v/v) dichlormethane: 1,2-dichloroethane mixture was employed as an extraction solvent and sprayed onto sample or standard solutions using a straightforward and practical spray apparatus. The factors affecting the extraction process such as extraction solvent type and ratio, extraction solvent volume (spray repetition), vortexing period, and sample pH were properly optimized. Analytical figures of the merit of the method were recorded under the optimal extraction/chromatographic conditions. The LOD, LOQ, and enhancement factor were in the range of 1.0 to 6.6 ng/g, 3.2 to 22.1 ng/g, and 3.7 to 158.9, respectively. The method demonstrated a good linear working range for all the selected analytes with proper coefficients of determination. The usability and reliability of the microextraction strategy was confirmed using seawater, moss, and soil samples, and the %recoveries were within an acceptable range (> 70%) for all examined samples. The environmental samples collected from the Horseshoe and Faure Islands of the Antarctica region were analyzed to assess the potential pollution of EDCs and pesticides. This method has the potential to be employed for the analysis of EDCs in routine analytical laboratories and for controlling and screening the organic pollutant content of different environmental samples.
Assuntos
Disruptores Endócrinos , Microextração em Fase Líquida , Praguicidas , Água/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Praguicidas/análise , Disruptores Endócrinos/análise , Regiões Antárticas , Microextração em Fase Líquida/métodos , Reprodutibilidade dos Testes , Solo , Solventes/químicaRESUMO
The endocrine-disrupting potential of parabens, as well as their relation to cancer, has sparked significant discussions over their impact. Consequently, analyses of cosmetic products are an essential necessity, particularly in terms of human health and safety. In this study, a highly accurate and sensitive liquid-phase-based microextraction method was developed to determine the five parabens at trace levels by high-performance liquid chromatography. All prominent parameters of the method such as extraction solvent type and amount (1,2-dichloroethane/250 µL), and dispersive solvent type and amount (isopropyl alcohol/2.0 mL) were optimized to enhance the extraction efficiency of the analytes. The mobile phase consisting of 50 mM ammonium formate aqueous solution (pH 4.0) and acetonitrile (60:40, v/v) was used to elute the analytes at a flow rate of 1.2 mL min-1 in the isocratic mode. Analytical performance of the optimum method for methyl, ethyl, propyl, butyl and benzyl parabens were determined and the analytes recorded detection limit values of 0.78, 0.75, 0.34, 0.33 and 0.75 µg kg-1, respectively. Four different lipstick samples were analyzed under optimum conditions of the developed method, and the amount of parabens quantified in the samples using matrix matched calibration standards was in the range of 0.11-1.03%.
Assuntos
Microextração em Fase Líquida , Parabenos , Humanos , Cromatografia Líquida de Alta Pressão , Parabenos/análise , Solventes/análise , Água/química , Microextração em Fase Líquida/métodosRESUMO
Rose tea infusion has gained popularity worldwide due to its health benefits. However, it is known that tea plants can be contaminated with heavy metals including copper. Hence, an accurate and applicable analytical method namely emulsification liquid-liquid microextraction based deep eutectic solvent - flame atomic absorption spectrometry (ELLME-DES-FAAS) was proposed to determine copper at trace levels in rose tea samples. Under the optimum experimental conditions, analytical figures of merit for the developed method were examined, and dynamic range, limit of detection (LOD) and limit of quantification (LOQ) were found to be 5.07-246.61 µg/kg (mass-based) with 0.9992 coefficient of determination, 2.50 µg/kg and 8.32 µg/kg, respectively. A matrix matching calibration strategy was employed to boost recovery results, and the acceptable recovery results were recorded between 95.9 % and 118.4 %. According to recovery results, the developed analytical method can be safely employed to determine the concentration of copper in rose tea samples accurately.
Assuntos
Microextração em Fase Líquida , Poluentes Químicos da Água , Cobre/análise , Microextração em Fase Líquida/métodos , Espectrofotometria Atômica/métodos , Análise de Alimentos/métodos , Solventes/química , Limite de Detecção , Chá/química , Poluentes Químicos da Água/análiseRESUMO
In the present study, a green and sensitive analytical method for the determination of copper ion at trace levels in apple tea samples was developed. Simultaneous complexation/extraction of the analyte were achieved by spraying-based fine droplet formation liquid-phase microextraction (SFDF-LPME). Copper ion was complexed with a Schiff base chelating agent called as N,N'-Bis(salicylidene)-1,2-phenylenediamine (BSP). Under the optimum conditions, the developed SFDF-LPME-FAAS and FAAS system were assessed with respect to limit of detection (LOD), limit of quantitation (LOQ), linearity and percent relative standard deviation (%RSD). LOD and LOQ values for SFDF-LPME-FAAS method were found to be 6.0 and 19.9 µg/kg, respectively. Enhancement in calibration sensitivity for developed method was found as 23 folds. In addition, accuracy/suitability of the developed SFDF-LPME-FAAS method were confirmed by spiking experiments. Two different apple tea samples were spiked to different concentration values and percent recovery results from 91.1 and 123.8 % proved the accuracy/suitability of the method.
Assuntos
Microextração em Fase Líquida , Malus , Cobre/análise , Espectrofotometria Atômica/métodos , Quartzo , Limite de Detecção , Microextração em Fase Líquida/métodos , CháRESUMO
This study employed simple polystyrene-coated magnetite nanoparticles (PS@MNPs)-assisted batch adsorption process for the removal of two antidepressant active ingredients (amitriptyline HCl and sertraline HCl) from hospital wastewater. Dominant parameters of the adsorption process including pH, adsorbent amount, and contact period were optimized through the univariate approach to enhance the adsorption efficiency. Upon reaching optimum adsorption conditions, equilibrium experiments were performed by spiking the adsorbates in hospital wastewater in the concentration range of 100-2000 µg/L. The concentrations of the adsorbates in the effluent were calculated using the matrix-matching calibration strategy to enhance the accuracy of quantification. A validated switchable solvent-based liquid phase microextraction (SS-LPME) method was employed to enrich the two active pharmaceutical ingredients (APIs) prior to sensitive determination with GC-MS (gas chromatography-mass spectrometry). The equilibrium data were mathematically modeled employing the Langmuir and Freundlich adsorption isotherm models. The isotherm constants were calculated, and the results showed that both the isotherm models fitted well with the experimental data. The efficient and simple batch adsorption strategy reported in this study was successfully employed to remove amitriptyline HCl and sertraline HCl from hospital wastewater at low concentrations.
Assuntos
Nanopartículas de Magnetita , Poluentes Químicos da Água , Amitriptilina/análise , Águas Residuárias , Princípios Ativos , Poliestirenos/análise , Sertralina/análise , Adsorção , Nanopartículas de Magnetita/química , Monitoramento Ambiental , Antidepressivos/análise , Poluentes Químicos da Água/análise , Cinética , Concentração de Íons de HidrogênioRESUMO
Despite the many benefits derived from the unique features and practicality of nanoparticles, the release of their toxic by-products or products from the synthesis stage into the environment could negatively impact natural resources and organisms. The physical and chemical methods for nanoparticle synthesis involve high energy consumption and the use of hazardous chemicals, respectively, going against the principles of green chemistry. Biological methods of synthesis that rely on extracts from a broad range of natural plants, and microorganisms, such as fungi, bacteria, algae, and yeast, have emerged as viable alternatives to the physical and chemical methods. Nanoparticles synthesized through biogenic pathways are particularly useful for biological applications that have high concerns about contamination. Herein, we review the physical and chemical methods of nanoparticle synthesis and present a detailed overview of the biogenic methods used for the synthesis of different nanoparticles. The major points discussed in this study are the following: (1) the fundamentals of the physical and chemical methods of nanoparticle syntheses, (2) the use of different biological precursors (microorganisms and plant extracts) to synthesize gold, silver, selenium, iron, and other metal nanoparticles, and (3) the applications of biogenic nanoparticles in diverse fields of study, including the environment, health, material science, and analytical chemistry.
Assuntos
Nanopartículas Metálicas , Nanoestruturas , Bactérias/química , Nanoestruturas/química , Fungos/química , Fungos/metabolismo , Prata/química , Ferro/metabolismo , Nanopartículas Metálicas/química , Extratos Vegetais/química , Química VerdeRESUMO
In this study, detection sensitivity of the conventional flame atomic absorption spectrophotometer (FAAS) for the determination of manganese (Mn2+) was enhanced by employing a preconcentration method from wastewater samples. Flower-shaped Ni(OH)2 nanomaterials were synthesized and used as sorbent material in preconcentration procedure. With the aim of attaining optimum experimental conditions, effective parameters of extraction method were optimized and these included pH of buffer solution, desorption solvent concentration and volume, mixing type and period, nanoflower amount, and sample volume. The detection limit of the optimized method was determined to be 2.2 µg L-1, and this correlated to about 41-fold enhancement in detection power relative to direct FAAS measurement. Domestic wastewater was used to test the feasibility of the proposed method to real samples by performing spike recovery experiments. The wastewater sample was spiked at four different concentrations of manganese, and the percent recoveries determined were in the range of 95-120%.
Assuntos
Manganês , Níquel , Níquel/análise , Manganês/análise , Águas Residuárias , Monitoramento Ambiental/métodos , Solventes , Espectrofotometria Atômica/métodosRESUMO
This study presents a highly sensitive and accurate analytical strategy for the determination of fenuron in wastewater samples using gas chromatography-mass spectrometry (GC-MS). Simultaneous derivatization and spray-based fine droplet formation-liquid phase microextraction (SFDF-LPME) method was developed and performed to achieve low detection limits. The parameters of the derivatization and SFDF-LPME method were optimized by univariate approach to improve sensitivity and selectivity. Under the optimum SFDF-LPME-GC-MS conditions, the limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.15 and 0.49 mg/kg, respectively. In addition, the linear range was calculated as 0.51-24.50 mg/kg. Recovery studies were carried out on wastewater samples to determine the accuracy of the developed method and its applicability to real sample matrix. Matrix matching calibration strategy was applied to eliminate/reduce any possible interference effects caused by the complexity of the wastewater matrix and to increase the accuracy of the analytical results. Percent recovery results varied between 85.9 and 120.9% with small percent relative standard deviation values. These results were satisfactory in terms of the accuracy and applicability of the proposed method for wastewater samples.
Assuntos
Monitoramento Ambiental , Águas Residuárias , Calibragem , Cromatografia Gasosa-Espectrometria de MassasRESUMO
The environmental impacts and risks of nanomaterials that are commonly used in different technologies are of great concern as their toxic effects on the aquatic ecosystem remain unclear. In this study, bismuth sulfide (Bi2S3) nanoflowers (nfs) were synthesized using a microwave-based hydrothermal process, and their genotoxic effects were investigated in the common carp, Cyprinus carpio. Bi2S3 nanoflowers were applied to common carp for 96 h. LC50 value (LC50 = 350 mg/L-1) was determined for acute toxicity with probit analysis, and three sublethal concentrations (35, 87, and 175 mg/L-1) were selected accordingly for genotoxicity tests. Such LC50 value - 350 mg L-1 for the common carp makes these nanoflowers non-toxic to aquatic organisms according to the EU-Directive 93/67/EEC classification scheme. Toxicological evaluations of the sublethal concentrations of Bi2S3 nanoflowers demonstrated that the 35 and 87 mg L-1 Bi2S3nfs groups were generally harmless and similar to the control group. Only the 175 mg L-1 Bi2S3nfs group had significant DNA damage frequency and nuclear abnormalities than the control and other Bi2S3nfs groups. To the best of our knowledge, this is a novel data on genotoxicity reported for fish species exposed to Bi2S3 nanoflowers; however, further systematic studies need to be performed to fully estimate the effects of Bi2S3 nanoflowers on aquatic life.
Assuntos
Carpas , Animais , Ecossistema , Monitoramento Ambiental , Dano ao DNARESUMO
In this study, a magnetic sorbent assisted dispersive solid phase extraction (DSPE) method was used to preconcentrate lead ions from rooibos tea samples for determination by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS). Cobalt ferrite magnetic nanoparticles (CoFe2O4 MNPs) were synthesized by microwave assisted digestion. Limits of detection and quantification were calculated as 5.3 and 17.6 µg/L, respectively, in a linear dynamic range of 20-800 µg/L. The enhancement factor of the developed method was found to be 80-folds when compared to the detection limit of the regular FAAS system. The percent recoveries obtained for rooibos tea samples spiked at different concentrations were in the range of 77 - 125%, with high repeatability as indicated by low standard deviations. The findings of the study demonstrated that the CoFe2O4 MNPs-based extraction method is a straightforward, fast, affordable, safe, and eco-friendly approach to qualifying/quantifying lead with high precision in the selected beverage sample.
Assuntos
Aspalathus , Microextração em Fase Líquida , Nanopartículas , Micro-Ondas , Microextração em Fase Líquida/métodos , Espectrofotometria Atômica/métodos , Chá/químicaRESUMO
Simple, inexpensive and accurate analytical methods are in high demand. Dispersive solid-phase microextraction (DSPME) was used in combination with smartphone digital image colorimetry (SDIC) to determine boron in nuts as an approach replacing existing costly alternatives. A colorimetric box was designed to capture images of standards and sample solutions. ImageJ software was used to link pixel intensity to the analyte concentration. Under optimum extraction and detection conditions, linear calibration graphs were obtained with coefficients of determination (R2) above 0.9955. Percentage relative standard deviations (%RSD) were below 6.8 %. The limits of detection (LOD) ranged between 0.07 and 0.11 µg mL-1 (1.8 to 2.8 µg g-1), which were sufficient for detection of boron in nut samples (i.e., almond, ivory, peanut and walnut), with percentage relative recoveries (%RR) between 92.0 and 106.0 %.
Assuntos
Colorimetria , Microextração em Fase Líquida , Colorimetria/métodos , Boro , Smartphone , Microextração em Fase Líquida/métodos , Microextração em Fase Sólida/métodos , Limite de DetecçãoRESUMO
In order to eliminate the effects of seawater matrix on the precise/accurate determination of elements, new and efficient analytical procedure requires. In this study, co-precipitation method based on the triethylamine (TEA)-assisted Mg(OH)2 was performed to eliminate side-effects of seawater medium on the determination with flame atomic absorption spectrometry (FAAS) prior to the preconcentration of nickel by an optimized dispersive liquid-liquid microextraction (DLLME) method. Under the optimum conditions of the presented method, the limit of detection and quantification (LOD, LOQ) values obtained for nickel were found as 16.1 and 53.8 µg kg-1, respectively. Seawater samples collected from West Antarctic region were used for real sample applications to check the accuracy and applicability of developed method, and satisfying recovery results (86-97%) were obtained. In addition to this, the digital image-based colorimetric detection system and the UV-Vis system were applied to confirm the applicability of the developed DLLME-FAAS method in other analytical systems.
Assuntos
Microextração em Fase Líquida , Níquel , Níquel/análise , Microextração em Fase Líquida/métodos , Monitoramento Ambiental/métodos , Água do Mar , Limite de Detecção , Espectrofotometria Atômica/métodosRESUMO
Aim: An accurate and sensitive analytical method was proposed to detect some steroid hormones in biological samples. Materials & methods: An Fe3O4/reduced graphene oxide nanocomposite-based dispersive solid-phase extraction was developed for the effective and simple preconcentration of steroid hormones from human serum samples. Results & conclusion: The nanocomposite was firstly used as adsorbent to simultaneously extract the selected hormones. Limit of detection values for the selected hormones were calculated between 5.5 and 39.2 ng/kg (mass based). An artificial serum sample was used to test the applicability and accuracy of the developed method; percentage recovery results obtained from two different spiked concentrations were found to be in the range of 80.5-99.9%.
Assuntos
Nanocompostos , Nanocompostos/química , Extração em Fase Sólida , Esteroides/química , Hormônios/química , HumanosRESUMO
In this study, a green, simple and effective preconcentration method named as spray-assisted fine droplet formation-liquid phase microextraction (SAFDF-LPME) before the flame atomic absorption spectrophotometry (FAAS) measurement for cobalt determination was developed. The method reduces the external dispersive solvent usage by using a simple spraying apparatus to obtain fine droplets of the extraction solvent. SAFDF-LPME method also consists of simultaneous complexation and extraction which indicates the environmental benevolence of the developed method. This method minimized the relative errors with high repeatability and accuracy by reducing the experimental steps. The influential parameters such as buffer type, buffer solution volume, extraction solvent/ligand solution volume (spraying cycle), and mixing period were systematically optimized by the univariate optimization procedure. With the optimum parameters applied, the detection power of the FAAS system was enhanced to about 110-folds with respect to 2.2 ng mL-1 detection limit calculated for the proposed method. Bottled drinking water samples from Fiji Islands were used to demonstrate the applicability of the developed method for the accurate determination of trace cobalt in real sample matrices. Percent recovery results obtained between 95.5 and 88.5% showed the suitability of the developed method in the determination of cobalt at trace levels even in complex sample matrices.
Assuntos
Água Potável , Microextração em Fase Líquida , Poluentes Químicos da Água , Espectrofotometria Atômica/métodos , Microextração em Fase Líquida/métodos , Cobalto/análise , Fiji , Quartzo , Limite de Detecção , Monitoramento Ambiental/métodos , Solventes , Poluentes Químicos da Água/análiseRESUMO
This study presents a simple, sensitive, and accurate method for the determination of nickel by flame atomic absorption spectrometry (FAAS). Prior to instrumental measurement, a deep eutectic solvent-based simultaneous complexation and preconcentration (DES-SCP) method was used to preconcentrate nickel from aqueous solution into measurable quantities. The efficiency of the extraction method was enhanced by forming a non-ionic complex of nickel using dithizone as ligand. By mixing the ligand with the DES extractant, simultaneous complexation and preconcentration of nickel were achieved in a single step. Under optimum conditions of the extraction method, the limit of detection (LOD) and the limit of quantification (LOQ) values were found to be 2.4 and 8.0 ng/mL, respectively. With respect to direct FAAS measurement, the developed method enhanced the sensitivity of nickel determination by about 169 folds. The accuracy and applicability of the developed method were evaluated by performing spike recovery experiments with lake water sampled from Antarctica. Satisfactory recovery results in the range of 94.0-113.7% were recorded and this validated the developed method as an efficient and green alternative for nickel determination.