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A new, simple and rapid spectrophotometric method was developed for determination of Sudan Black B in food products by supramolecular solvent-based-vortex-assisted-dispersive liquid liquid microextraction (SUPRAS-VA-DLLME). Extraction solvent type, volume of solvent, pH, volume of THF, centrifugation time, vortex time, and sample volume were investigated as optimization parameters of the developed method. Under the optimum conditions, limit of detection and limit of quantification, preconcentration factor and enhancement factor of the developed method were calculated to be 9.01 µg L-1, 29.73 µg L-1, 20, and 55, respectively. The developed microextraction method was successfully applied to food samples for the determination of Sudan Black B.
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The aim of this study was to develop a practical orbital shaker-assisted magnetic solid phase extraction (OSA-MSPE) method for the determination of lead by FAAS. A new magnetic poly linoleic acid-polystyrene-polydimethylsiloxane (PSt-PLina-PDMS) hydrophobic graft copolymer was synthesized and characterized by NMR, FT-IR, SEM-EDX, DSC, TGA, BET and used as adsorbent for the extraction of Pb (II). This adsorbent can be used at least 50 times without any decrease of its adsorption properties for the adsorption and elution of analyte ions. Several analytical parameters including pH, adsorbent amount, sample volume, shaking time, etc. were optimized. Multivariate optimization was used for the investigation of different parameters. The linear range at optimum operating condition was 1.7-84 µg L-1. The limit of detection (LOD) and limit of quantification (LOQ) were 0.5 µg L-1, 1.7 µg L-1, respectively. Intraday and interday relative standard deviation (RSD %), enhancement factor (EF) and adsorbent capacity were found as 1.9%, 3.3%, 166.7, 50 mg g-1, respectively. OSA-MSPE method was tested with certified reference materials including LGC-6010 (Hard Drinking Water), NCS ZC73032 Celery and CS-M-3 Control Sample Microelements in Mushroom Powder for the accuracy. Experimental results for lead were confirmed with certified values. Present method was successfully applied to various liquid and solid food samples. The OSA-MSPE method has some important features such as selective, sensitive, low LOD, LOQ and RSD, pre-concentration factor (PF) and high enhancement factor (EF). High tolerance limits against matrix ions were achieved.
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Contaminação de Alimentos , Chumbo , Poliestirenos , Extração em Fase Sólida , Poluentes Químicos da Água , Extração em Fase Sólida/métodos , Extração em Fase Sólida/instrumentação , Contaminação de Alimentos/análise , Chumbo/isolamento & purificação , Chumbo/análise , Chumbo/química , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação , Poliestirenos/química , Adsorção , Polímeros/química , Ácido Linoleico/análise , Ácido Linoleico/isolamento & purificação , Ácido Linoleico/química , Dimetilpolisiloxanos/química , Limite de DetecçãoRESUMO
A new magnetic nano gel (MNG) was prepared from choline chloride/phenol deep eutectic solvent and magnetic amberlite XAD-7 nanocomposite. The dispersive solid phase micro extraction (dSPME) method was developed for seperation and preconcentration of Brilliant Blue FCF (BB) by the prepared MNG. In this study, firstly, the optimum DES type and mole ratio of DES were investigated before response surface methodology optimization. Then, the effect of the MNG-dSPME experimental parameters were optimized by response surface methodology using central composite design. Under the optimum microextraction conditions, limit of detection (LOD), limit of quantification (LOQ), preconcentration factor (PF), enhencament factor (EF) were found to be 1.15 µg L-1,3.80 µg L-1, 70, and 88, respectively. It was seen that the recovery of real samples were obtained from 95.5 to 103.6%. The pesent method was succesfully for extraction of BB in some food, personal care samples, to the best of our knowledge, this is the first study that is presented method on determination of BB by preconcentration with magnetic nano gel. The obtained results showed that the present procedure is effective, sensitive, and has high accuracy for the quantitative detection of BB.
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Solventes Eutéticos Profundos , Contaminação de Alimentos , Limite de Detecção , Microextração em Fase Sólida , Contaminação de Alimentos/análise , Microextração em Fase Sólida/métodos , Microextração em Fase Sólida/instrumentação , Solventes Eutéticos Profundos/química , Espectrofotometria , Benzenossulfonatos/químicaRESUMO
A new graft copolymer composed of polystyrene and polylinoleic acid (PLinas) with the sodium salt of iminodiacetate (Ida) was synthesized and used as an adsorbent. The vortex-assisted dispersive solid-phase micro-extraction (VA-dSPµE) method was used for the extraction and pre-concentration of chromium. Multivariate methodologies, such as factorial design and 3D surface plots, were applied for screening and optimizing effective extraction parameters. The influence of diverse analytical parameters, such as pH, sample volume, and interfering ions, on the extraction of chromium was studied. The calibration standard curve exhibited a linear range from 0.01 to 0.50 µg L-1. The relative standard deviation and limit of detection were found to be 1.65 % and 0.003 µg L-1, respectively. Extraction recoveries were found in the range of 96 to 99 % by using certified reference materials (CRMs). The adsorbent capacity of PLinas-Ida was found to be 112 mg g-1. The VA-dSPµE method demonstrated its effectiveness in the pre-concentration and determination of chromium within samples of foodstuffs by graphite furnace-atomic absorption spectrometry (GF-AAS).
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Cromo , Extração em Fase Sólida , Extração em Fase Sólida/métodos , Polímeros/química , Microextração em Fase Sólida/métodos , Espectrofotometria Atômica/métodosRESUMO
Background: Cadmium (Cd) is a very toxic and carcinogenic heavy metal even at low levels and it is naturally present in water as well as in food. Methods: A new polyvinyl benzyl xanthate (PvbXa) was synthesized and used as a new adsorbent in this work. It contains pendant sulfide groups on the main polystyryl chain. Using this new adsorbent, PvbXa, a vortex-assisted dispersive solid-phase microextraction (VA-dSPµE) procedure was developed for the determination of cadmium from food and water samples via flame atomic absorption spectrophotometry (FAAS). Synthesized PvbXa was characterized by 1H Nuclear magnetic resonance (NMR) Spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). The different parameters of pH, sample volume, mixing type and time, sorbent amount, and eluent time were optimized using standard analytical methods. Results: The optimized method for assessment of Cd in food and water samples shows good reliability. The optimum conditions were found to be a 0.20-150 µg L-1 linear range, 0.06 µg L-1 LOD, 0.20 µg L-1 LOQ, 4.3 RSD %, and a preconcentration factor of 160. Conclusions: The statistically experimental variables were utilized using a central composite design (CCD). The present method is a low-cost, simple, sensitive, and very effective tool for the recovery of Cd.
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In the current study, salt- and pH-induced homogeneous dispersive solid phase extraction was developed using albumin as a sorbent for the extraction of some pesticides (diazinon, diniconazole, haloxyfop-R-methyl, and hexaconazole) from fruit juice of orange, pomegranate, and barberry. The extracted analytes were more concentrated by dispersive liquid-liquid microextraction to obtain high enrichment factors and low detection limits prior to their determination by gas chromatography-mass spectrometry. In the extraction process, human serum albumin solution was added to the sample solution at the µL-level and a homogeneous solution was obtained. Then, albumin was precipitated into the solution by adding an inorganic salt and decreasing the solution pH. By doing so, the analytes were adsorbed by albumin effectively due to their high adsorption capacity and large surface area. Following this, the pesticides were eluted from the albumin sorbent using an elution solvent and used in a dispersive liquid-liquid microextraction step. Under the optimum extraction conditions, low limits of detection and quantification were achieved in the ranges of 0.02-0.04 and 0.07-0.13 ng mL-1, respectively. The calibration curves were linear in the range of 0.13-250 ng mL-1. Relative standard deviation as a criterion for precision and the method repeatability were in the ranges of 2.9-4.2% for intra- (n = 5, C = 5 or 50 ng mL-1) and 3.2-5.2% for inter-day (n = 5, 50 ng mL-1) precisions. The enrichment factors and extraction recoveries were in the ranges of 390-460 and 78-92%, respectively. Finally, the offered procedure was applied for the analysis of pesticide residues in some fruit juice samples.
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Resíduos de Praguicidas , Praguicidas , Humanos , Praguicidas/análise , Sucos de Frutas e Vegetais/análise , Resíduos de Praguicidas/análise , Cloreto de Sódio/análise , Extração em Fase Sólida/métodos , Cloreto de Sódio na Dieta/análise , Albuminas/análiseRESUMO
A new polyoleic acid-polystyrene (PoleS) block/graft copolymer was synthesized and applied as adsorbent for ultrasound assisted dispersive solid phase microextraction (UA-DSPME) of Sb(III) in different bottled beverages and analysis using hydride generation atomic absorption spectrometry (HGAAS). Adsorption capacity of the PoleS was 150 mg g-1. Several sample preparation parameters such as sorbent amount, solvent type, pH, sample volume and shaking time were optimized (based on central composite design (CCD) approach) and evaluated in respect to the recovery of Sb(III). The method revealed a high tolerance limit of matrix ions presence. Under optimized conditions, linearity range, the limit of detection, the limit of quantitation, extraction recovery, enhancement factor, preconcentration factor were 5-800 ng L-1, 1.5 ng L-1, 5.0 ng L-1, 96%, 82, 90, respectively. Accuracy of the UA-DSPME method was confirmed based on different certified reference materials and standard addition method. Factorial design was utilized to estimate the influences of variables of recovery of Sb(III).
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Microextração em Fase Líquida , Microextração em Fase Sólida , Microextração em Fase Sólida/métodos , Poliestirenos/química , Espectrofotometria Atômica/métodos , Bebidas/análise , Polímeros/análise , Limite de DetecçãoRESUMO
As a novel adsorbent, an opioid silver-morphine-functionalized polypropylene was synthesized through a one-pot reaction at room temperature and successfully used for the simple one-pot photocatalytic degradation catalyst of methyl orange removal from wastewater. UV spectral analysis reveals a special reference to the excitation of surface plasmon resonance as the main characteristic of the polymer-Ag nanocomposite in toluene solution peak at 420 nm in AgPP-mrp catalyst. The 1H NMR spectrum showed no sign of Ag NP peaks revealing small size distribution in the channels of morphine-functionalized polypropylene polymer. The morphology of silver nanoparticle-doped polymer through scanning electron microscopy (SEM-EDX) reveals PP-mrp with continuous matrix and Ag NPs (0.87 wt%). Furthermore, photocatalytic degradation of methyl orange was investigated on AgPP-mrp catalyst spectrophotometrically under solar irradiation in waste effluent, demonstrating high degradation efficiency. According to experimental findings, silver nanoparticles (AgPP-mrp) achieved high degradation capacities of 139 mg/g equivalent to 97.4% of photodegradation in a little period of time (35 min), as associated with previously stated materials and follow pseudo-second-order kinetic degradation tail of a high regression coefficient (R2 = 0.992). The suggested techniques offer a linear reaction for MO over the pH range of 1.5 to 5 and a degradation temperature of 25 to 60 °C. Central composite design and response surface methodology statistics recommend pH of the reaction medium and time as important variables for methyl orange degradation on AgPP-mrp photocatalytic. AgPP-mrp on the photocatalytic phenomenon based on heterojunction catalytic design producing electron holes (e-), as well as superoxides for the successful degradation of methyl orange.
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Nanopartículas Metálicas , Nanocompostos , Nanopartículas Metálicas/química , Prata/química , Polipropilenos , Morfina , Nanocompostos/química , CatáliseRESUMO
Liquid phase microextraction techniques are considered as the miniaturized version of traditional liquid-liquid extraction, which use only several microliters of a proper solvent to extract the analytes from sample. In these methods, the target analytes are migrated into a water-immiscible organic solvent (acceptor phase) from an aqueous sample (donor phase). They are mainly classified into three main groups including (a) single-drop microextraction, (b) dispersive liquid-liquid microextraction, and (c) hollow fiber-liquid phase microextraction. These techniques have been successfully applied to the assessment of different analytes in food samples, pharmaceuticals, beverages, and so on. This review mainly focuses on up-to-date information on the application of liquid phase microextraction techniques in dairy products. The advantages and disadvantages of the developed liquid phase microextraction methods were discussed.
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Green solvents (GSs) has gained significant attention in recent years due to their potential as safer and more sustainable alternatives to traditional organic solvents. Solvents are used in a wide range of applications, from industrial processes to everyday products. Solvent emissions and losses can have a significant impact on the environment and human health, which is why many initiatives are being undertaken to get rid of or switch to eco-friendly alternatives. A key area of green chemistry that led to the concept of "green" solvents is the development of alternative solvents that are less toxic and more environmentally friendly than traditional organic solvents. The advantages of using green solvents over conventional ones are their environmental friendliness, biocompatibility, biodegradability, and simplicity of preparation. Different sample preparation techniques have successfully utilized green solvents to offer a sustainable separation media for the extraction of a variety of inorganic and organic compounds which are crucial for research in environmental samples. Recent developments in green analytical chemistry (GAC) have focused on how to prepare and use samples using environmentally sustainable solvents. The current study covers the advance and currently used green solvents with an emphasis on environmentally friendly sample preparation methods. This review aims to briefly summarize the current state of knowledge about the use of green solvents particularly ionic liquids, deep eutectic solvents and switchable solvents (SSs) with the perspective of GAC in sample preparation methods.
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A sensitive and robust trap method was developed for the determination of cadmium (Cd) by using a slotted quartz tube. Using this method at a sample suction rate of 7.4 mL/min for 4.0 min collection, a 1467-fold increase in sensitivity was obtained compared to the flame atomic absorption spectrometry method. Under the optimized conditions, a limit of detection of 0.075 ng mL-1 was obtained for the trap method. The interference effects of hydride-forming elements, transition metals, and some anions on the Cd signal were investigated. The developed method was evaluated by analyzing "Sewage Sludge-industrial origin (BCR no: 146R)", "NIST SRM 1640a Trace elements in natural water", and "DOLT: 5 Dogfish Liver". There was a good agreement between the certified and found values at the 95% confidence level. This method was applied successfully for the determination of Cd in drinking water and some fish tissue samples (liver, muscle, and gill) obtained from Mugla province.
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Simple, rapid, low cost, selective, and sensitive analytical method was developed using fatty acid-based ternary deep eutectic solvents (TDESs) for extraction and determination of tetracycline in honey, milk and water samples by vortex assisted (VA) microextraction and UV-vis spectrophotometer. Four different TDES were prepared by combination of nonanoic acid, dodecanoic acid, decanoic, hexanoic acid, octanoic acid. Analytical parameters such as pH, TDES types and its molar ratio, dispersive solvent types and solvent volume and salt effect were optimized. VA-TDES method was good recovery of tetracycline in the samples from 94 to 99%. The LOD and LOQ values were found 1.0 and 3.3 µg L-1, respectively. The linear range of calibration graph was 3.3 -450 µg L-1. Intra-day and inter-day precision was found 2.8-4.1% and 3.6-5.2%. Enhancement factor was found 109. The factorial design was drawn to evaluate the significant level of factors and effects of variables on the recovery of tetracycline. Standard addition method was used for the validation and accuracy of the method. Present VA-TDES method was successfully applied to real samples.
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Mel , Microextração em Fase Líquida , Animais , Solventes Eutéticos Profundos , Ácidos Graxos/análise , Mel/análise , Limite de Detecção , Microextração em Fase Líquida/métodos , Leite/química , Solventes/química , Tetraciclina/análise , Água/químicaRESUMO
Selenium (Se) is considered to be an essential trace element needed for all living organisms. The importance, deficiency, and toxic effects of Se mainly depend on its quantity and chemical nature. It has been observed that the inorganic versions of Se are more hazardous than the organic versions. This review is mainly focused on the application of different extraction methods used for Se extraction and determination such as microextraction, solid-phase extraction (SPE), and their modified modes in the last 12 years. The use of different dispersive medium (magnetic field, ultrasonic radiation, and vortex agitator) to enhance Se separation is also part of this review. The usage of environmentally friendly solvents such as supramolecular solvents, hydrophobic deep eutectic solvents (DESs), and ionic liquids (ILs) are also the focus of attention in this review. This review is also emphasized the application of advanced microextraction methods, particularly liquid-phase microextraction (LPME). The most recent advances in LPME extraction techniques for Se in various environmental samples, as well as their prospects, are reviewed. Additionally, a summary of cheap, simple, and accurate techniques that have not yet been used to determine small amounts of Se has been provided.
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A green and innovative ultrasonic-assisted dispersive liquid-liquid microextraction using hydrophilic deep eutectic solvents (UA-HDES-DLLME) was developed for the selective and simultaneous extraction and enrichment of Pb (II) and Cd (II) in water and food samples for flame atomic absorption spectrometry. Several natural deep eutectic solvents (NADES) were used for the preparation of six different HDES and methyl violet was used as chelating reagent. Effective parameters such as pH, sonication time, methyl violet amount, DES type, dispersive solvent types, etc were optimized. Relative standard deviation (RSD) and preconcentration factor (PF) were 4.0% and 80. Low limits of detection (LOD, 1.3 ng mL-1 for Pb (II) and 0.33 ng mL-1 for Cd (II)) and quantification (LOQ, 4.0 ng mL-1 for Pb (II) and 1.0 ng mL-1 for Cd (II)) were found. The method accuracy was confirmed with analyses of certified reference materials.
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Microextração em Fase Líquida , Microextração em Fase Líquida/métodos , Cádmio/análise , Água/química , Solventes Eutéticos Profundos , Violeta Genciana/análise , Limite de Detecção , Solventes/químicaRESUMO
Sample preparation is one of the viable procedures to be used before analysis to enhance sensitivity and reduce the matrix effect. The current review is mainly emphasized the latest outcome and applications of microextraction techniques based on the miniaturization of the classical conventional methods based on liquid-phase and solid-phase extraction for the quantitative elemental analysis in different real samples. The limitation of the conventional sample preparation methods (liquid and solid phase extraction) has been overcome by developing a new way of reducing size as compared with the conventional system through the miniaturization approach. Miniaturization of the sample preparation techniques has received extensive attention due to its extraction at microlevels, speedy, economical, eco-friendly, and high extraction capability. The growing demand for speedy, economically feasible, and environmentally sound analytical approaches is the main intention to upgrade the conventional procedures apply for sample preparation in environmental investigation. A growing trend of research has been perceived to quantify the trace for elemental analysis in different natures of real samples. This review also recapitulates the current futuristic scenarios for the green and economically viable procedure with special overemphasis and concentrates on eco-friendly miniaturized sample-preparation techniques such as liquid-phase microextraction (LPME) and solid-phase microextraction (SPME). This review also emphasizes the latest progress and applications of the LPME and SPME approach and their future perspective.
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Deep eutectic solvents (DESs) have been developed as green solvents and these are capable as alternatives to conventional solvents used for the extraction of organic and inorganic species from food and water samples. The continuous generation of contaminated waste and increasing concern for the human health and environment have compelled the scientific community to investigate more ecological schemes. In this concern, the use of DESs have developed in one of the chief approach in the field of chemistry. These solvents have appeared as a capable substitute to conventional hazardous solvents and ionic liquids. The DESs has distinctive properties, easy preparation and components availability. It is not only used in scienctific fields but also used in quotidian life. There are many advantages of DESs in analytical chemistry, they are largely used for extraction and determination of inorganic and organic compounds from different samples. In previous a few years, several advanced researches have been focused on the separation and preconcentration of low level of pollutants using DESs as the extractants. This review summarizes the use of DESs in the separation and preconcentration of organic and inorganic species from water and food samples using various microextraction processes.
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A new and novel poly(vinyl benzyl dithiocarbonate-dimethyl amino ethyl methacrylate) block copolymer (Pvb-DMA-Xa) as adsorbent was synthesized for the vortex-assisted dispersive solid phase microextraction (VA-DSPME) of patulin from apple products and dried fruits using Uv-visible spectrophotometer. The characterization of synthesized Pvb-DMA-Xa block copolymer was performed with Fourier Transform Infrared spectroscopy (FTIR-ATR) technique. Analytical characteristics such as pH, sorbent amount, adsorption time, eluent type and its volume, desorption time and adsorption capacity were optimized. Limit of detection (3Sb/m) and limit of quantitation (10Sb/m) were found 0.3 and 1.0 ng mL-1. Linear dynamic range (LDR), relative standard deviation (RSD) and recovery values were found in the range of 1-30 ng mL-1, 2.1-2.7 % and 93.5-97.3 %, respectively. Enhancement factor (EF) was found 193. The accuracy of the method was confirmed with standard addition method and analyzing of samples by reference method.
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Malus , Patulina , Frutas/química , Limite de Detecção , Malus/química , Metacrilatos , Patulina/análise , Polímeros/química , Microextração em Fase Sólida/métodosRESUMO
A newly synthesized xanthate functionalized chlorinated polypropylene (PP-Xa) was used as adsorbent for the orbital shaker based on dispersive solid phase microextraction (OS-DSPME) of caffein from several tea, coffee, energy drink, coca-cola and chocolate samples using UV-vis. spectrophotometer. Synthesized PP-Xa was characterized using Fourier Transform Infrared spectroscopy (FTIR-ATR) and nuclear magnetic resonance spectroscopy (1H NMR). Various parameters like pH, PP-Xa amount, extraction time, type of eluent and its volume were optimized. Linear range, detection limit (LOD), limit of quantification (LOQ), relative standard deviation (RSD), recovery values, and enrichment factor (EF) were found 90-1000 µgL-1, 27.3 µg L-1, 90 µg L-1, 1.9-2.6%, 98 ± 2%, and 167, respectively. Adsorption capacity of PP-Xa was found 271.9 mg g-1. Standard addition and reference method were used for confirm the accuracy of present method.
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Cafeína , Microextração em Fase Sólida , Bebidas/análise , Limite de Detecção , Polipropilenos , Extração em Fase Sólida/métodos , Microextração em Fase Sólida/métodosRESUMO
An organic polymer was re-precipitated in solution to use as an adsorbent in dispersive solid-phase extraction of some pesticides from honey samples prior to their determination by high-performance liquid chromatography-tandem mass spectrometry. In this approach, different deep eutectic solvents were prepared using lysine and their ability in elution of the analytes from the adsorbent surface was tested. A diluted honey solution was transferred into a glass test tube and then a solution of polystyrene dissolved in dimethylformamide was injected into the solution. By doing this, polystyrene is re-precipitated in the solution and dispersed in whole parts of it as many tiny particles. Then the mixture was centrifuged and the adsorbed analytes on the particles were eluted using a proper hydrophilic deep eutectic solvent. The central composite design approach was used for the optimization of effective parameters. The limits of detection and quantification were in the ranges of 0.06-0.20 and 0.22-0.69 ng/g, respectively. The calibration curves obtained by matrix-matched standard solutions were linear in the range of 0.69-500 ng/g with a coefficient of determinations ≥0.9962. The method provided high extraction recoveries (70-99%) and enrichment factors (140-198), and an acceptable precision (relative standard deviations ≤7.1%).
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Mel , Microextração em Fase Líquida , Praguicidas , Mel/análise , Microextração em Fase Líquida/métodos , Praguicidas/análise , Poliestirenos , Extração em Fase Sólida/métodos , Solventes/químicaRESUMO
A dispersive solid-phase extraction method based on a new sorbent has been performed on plasma and wastewater samples to determine metoprolol by high-performance liquid chromatography-tandem mass spectrometry. In this study, the analyte was adsorbed from the samples onto microcrystalline cellulose as a green and efficient sorbent and then eluted for use in the determination step. In the mass spectrometer, the analyte was detected in the positive mode and selectivity of the analysis was increased by sequential mass analysis through multiple reaction monitoring. All of the effective parameters in the extraction of metoprolol from plasma and wastewater were optimized. Under optimal conditions the method was linear in the ranges of 1-1,000 and 0.1-1,000 ng/ml in plasma and wastewater samples, respectively. The detection limits of the method were 0.30 and 0.03 ng/ml in plasma and wastewater samples, respectively. The data showed that the method provides low detection limit, wide linear range, good precision and high extraction recovery. Finally several plasma and wastewater samples were successfully analyzed using the method. The use of a small amount of a green and inexpensive sorbent and a low volume of plasma without the need for further pretreatment steps are the main advantages of the method.