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1.
J Sep Sci ; 47(5): e2300070, 2024 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-38466171

RESUMEN

Herein, a deep eutectic solvent (DES)-based miniaturized pressurized liquid extraction in combination with DES-based dispersive liquid-liquid microextraction (DLLME) was developed for the extraction of organophosphorus pesticides (parathion-methyl, triazophos, parathion, diazinon, and phoxim) from egg powder samples prior to their analysis by a high-performance liquid chromatography-diode array detector. In this work, first, the analytes' extraction was done by a pressurized liquid phase extraction for effective extraction of the analytes from the solid matrix, and then they were concentrated on a DLLME for more concentration of the analytes to reach low limits of detections. The use of DESs was done in both steps to omit the use of toxic organic solvents. Satisfactory results including high extraction recoveries (74-90%), great repeatability (relative standard deviations equal or less than 4.3% and 5.3% for intra- and inter-day precisions), and low limits of detection (0.11-0.29 ng/g) and quantification (0.38-0.98 ng/g) were attained under the optimum conditions. Lastly, the suggested approach was utilized for the determination of the studied pesticides in various egg powder samples marketed in Tabriz, Iran.


Asunto(s)
Microextracción en Fase Líquida , Paratión , Residuos de Plaguicidas , Plaguicidas , Compuestos Organofosforados , Cromatografía Líquida de Alta Presión , Disolventes Eutécticos Profundos , Polvos
2.
J Pharm Pharm Sci ; 26: 11466, 2023.
Artículo en Inglés | MEDLINE | ID: mdl-37206631

RESUMEN

Purpose: An efficient, cost-effective and non-invasive test is required to overcome the challenges faced in the process of bioequivalence (BE) studies of various orally inhaled drug formulations. Two different types of pressurized meter dose inhalers (MDI-1 and MDI-2) were used in this study to test the practical applicability of a previously proposed hypothesis on the BE of inhaled salbutamol formulations. Methods: Salbutamol concentration profiles of the exhaled breath condensate (EBC) samples collected from volunteers receiving two inhaled formulations were compared employing BE criteria. In addition, the aerodynamic particle size distribution of the inhalers was determined by employing next generation impactor. Salbutamol concentrations in the samples were determined using liquid and gas chromatographic methods. Results: The MDI-1 inhaler induced slightly higher EBC concentrations of salbutamol when compared with MDI-2. The geometric MDI-2/MDI-1 mean ratios (confidence intervals) were 0.937 (0.721-1.22) for maximum concentration and 0.841 (0.592-1.20) for area under the EBC-time profile, indicating a lack of BE between the two formulations. In agreement with the in vivo data, the in vitro data indicated that the fine particle dose (FPD) of MDI-1 was slightly higher than that for the MDI-2 formulation. However, the FPD differences between the two formulations were not statistically significant. Conclusion: EBC data of the present work may be considered as a reliable source for assessment of the BE studies of orally inhaled drug formulations. However, more detailed investigations employing larger sample sizes and more formulations are required to provide more evidence for the proposed method of BE assay.


Asunto(s)
Albuterol , Nebulizadores y Vaporizadores , Humanos , Proyectos Piloto , Equivalencia Terapéutica , Administración por Inhalación
3.
J Sep Sci ; 46(20): e2300149, 2023 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-37712114

RESUMEN

Herein, a modified quick, easy, cheap, effective, rugged, and safe extraction was developed based on deep eutectic solvent for the extraction of several pesticides from canola oil samples. In this work, first, different sorbents were selected to remove the sample interferences, and the composition of the sorbents was optimized by simplex centroid design. The extracted analytes were more concentrated by solidification of floating deep eutectic solvent droplet-dispersive liquid-liquid microextraction. Low limits of detection (0.15-0.23 ng/g) and quantification (0.49-0.76 ng/g), high extraction recoveries (74-87%) and enrichment factors (224-263), and good repeatability (relative standard deviation equal to or less than 5.1 and 4.7% for intra- and interday precisions, respectively) were achieved using the proposed method. The suggested approach was used for the quantification of the analytes in different canola oil samples. Additionally, the effects of microwave irradiations exposure and sonication in decontamination of the samples were evaluated. In this method, there was no need for centrifugation and toxic solvents. Also, effective extraction of the analytes and minimizing interferences were achieved through the use of various sorbents.

4.
J Sep Sci ; 46(8): e2200696, 2023 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-36859691

RESUMEN

In this work, for the first time, a polymeric composite based on ß-cyclodextrin grafted with polyethylene has been prepared through ball milling and used as an efficient sorbent for dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffraction, and scanning electron microscopy. In the extraction process, after precipitating the proteins, the sorbent was added into the sample solution, and the mixture was vortexed to facilitate and speed up the sorption of the analytes onto the sorbent surface. After centrifuging, the sorbent particles were contacted with methanol to elute the analytes under the vortexing process. After this step, an aliquot of the eluate was taken and injected into high-performance liquid chromatography-diode array detector for quantitative analysis. Under the optimum extraction conditions, the extraction recoveries for metronidazole and clarithromycin were 76 and 83%, respectively. The limits of detection were 2.6 and 2.2 ng/ml for metronidazole and clarithromycin, respectively. The repeatability of the offered approach, expressed as relative standard deviation, was equal to or less than 4.7%. Finally, the method was successfully applied to plasma samples of the patients treated with metronidazole and clarithromycin.


Asunto(s)
Ciclodextrinas , beta-Ciclodextrinas , Humanos , Polietileno , Claritromicina , Metronidazol , Polímeros , Extracción en Fase Sólida/métodos , Límite de Detección
5.
J Sep Sci ; 46(10): e2200893, 2023 May.
Artículo en Inglés | MEDLINE | ID: mdl-36864003

RESUMEN

In the present work, a combination of microwave-assisted extraction with magnetic ionic liquid-based dispersive liquid-liquid microextraction was developed for the extraction of chloramine-T from fish samples. In this method, the sample was mixed with a hydrochloric acid solution and exposed to microwave irradiations. By doing so, chloramine-T was converted to p-toluenesulfonamide and extracted from the sample into an aqueous phase. Then, a mixture of acetonitrile (as a dispersive solvent) and magnetic ionic liquid (as an extraction solvent) was rapidly injected into the obtained solution. In the following, the magnetic solvent droplets including the extracted analytes were isolated from the aqueous solution in the presence of an external magnetic field and after diluting with acetonitrile injected into high-performance liquid chromatography equipped with a diode array detector. Under the optimum extraction conditions, high extraction recovery (78%), low limits of detection (7.2 ng/g) and quantification (23.9 ng/g), good repeatability (relative standard deviations ≤5.8 and 6.8% for intra- and inter-day precisions, respectively), and wide linear range (23.9-1000 ng/g) were obtained. Finally, various fish samples marketed in Tabriz city (East Azarbaijan, Iran) were analyzed with the suggested method.


Asunto(s)
Líquidos Iónicos , Microextracción en Fase Líquida , Animales , Cromatografía Líquida de Alta Presión , Microondas , Acetonitrilos , Peces , Iones , Solventes
6.
J Sep Sci ; 46(16): e2300068, 2023 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-37407502

RESUMEN

In this study, for the first time, a deep eutectic solvent-based microwave-assisted extraction was combined with ionic liquid-based temperature controlled liquid phase microextraction for the extraction of several aflatoxins from cheese samples. Briefly, the analytes are extracted from cheese sample (3 g) into a mixture of 1.5 mL choline chloride:ethylene glycol deep eutectic solvent and 3.5 mL deionized water by exposing to microwave irradiations for 60 s at 180 W. The liquid phase was taken and mixed with 55 µL 1-hexyl-3-methylimidazolium hexafluorophosphate. By cooling the solution in the refrigerator centrifuge, a turbid state was obtained and the analytes were extracted into the ionic liquid droplets. The analytes were determined by high-performance liquid chromatography equipped with fluorescence detector. Low limits of detection (9-23 ng kg-1 ) and quantification (30-77 ng kg-1 ), high extraction recovery (66%-83%), acceptable enrichment factor (40-50), and good precision (relative standard deviations ≤ 5.2%) were obtained using the offered approach. These results reveal the high extraction capability of the method for determination of aflatoxins in the cheese samples. In this method, there was no need for organic solvents and it can be considered as green extraction method.


Asunto(s)
Queso , Líquidos Iónicos , Microextracción en Fase Líquida , Microextracción en Fase Líquida/métodos , Disolventes Eutécticos Profundos , Microondas , Temperatura , Solventes/química , Límite de Detección
7.
J Sep Sci ; 46(13): e2200889, 2023 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-37058712

RESUMEN

An in-situ formed polymer-based dispersive solid phase extraction in combination with solidification of floating organic droplet-based dispersive liquid-liquid microextraction was developed for the extraction of neonicotinoid pesticides from milk samples. The extracted analytes were determined using high-performance liquid chromatography-diode array detector. In this approach, after precipitating the proteins of milk using a zinc sulfate solution, the supernatant phase (containing sodium chloride) was transferred into another glass test tube, and a homogenous solution of polyvinylpyrrolidone and a suitable water-miscible organic solvent was rapidly injected into it. By this step, the polymer particles were re-produced and the analytes were extracted onto the sorbent surface. In the following step, the analytes were eluted with an appropriate organic solvent to use in the following solidification of floating organic droplet-based dispersive liquid-liquid microextraction step that was done to acquire the low limits of detection. Under the optimized conditions, satisfactory results consisting of low limits of detection (0.13-0.21 ng/ml) and quantification (0.43-0.70 ng/ml), high extraction recoveries (73%-85%), and enrichment factors (365-425), and good repeatability (relative standard deviations equal or less than 5.1% and 5.9% for intra- and inter-day precisions, respectively) were obtained.


Asunto(s)
Microextracción en Fase Líquida , Plaguicidas , Animales , Plaguicidas/análisis , Neonicotinoides , Polímeros , Microextracción en Fase Líquida/métodos , Leche/química , Extracción en Fase Sólida/métodos , Solventes
8.
J Sep Sci ; 46(17): e2201055, 2023 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-37387553

RESUMEN

This research aims to synthesize a specific and efficient sorbent to use in the extraction of apixaban from human plasma samples and its determination by high-performance liquid chromatography-tandem mass spectrometry. High specific surface area of metal-organic framework, magnetic property of iron oxide nanoparticles, selectively of molecular imprinted polymer toward the analyte, and the combination of dispersive solid-phase extraction method with a sensitive analysis system provided an efficient analytical method. In this study, first, a molecularly imprinted polymer combined with magnetic metal organic framework nanocomposite was prepared and then characterized using different techniques. Then the sorbent particles were used for selective extraction of the analyte from plasma samples. The efficiency of the method was improved by optimizing effective parameters. According to the validation results, wide linear range (1.02-200 ng mL-1 ), acceptable coefficient of determination (0.9938), low limit of detection (0.32 ng mL-1 ) and limit of quantification (1.02 ng mL-1 ), high extraction recovery (78%), and good precision (relative standard deviations ≤ 2.9% for intra- (n = 6) and interday (n = 6) precisions) were obtainable using the proposed method. These outcomes showed the high potential of the proposed method for screening apixaban in the human plasma samples.


Asunto(s)
Estructuras Metalorgánicas , Impresión Molecular , Humanos , Polímeros Impresos Molecularmente , Microextracción en Fase Sólida/métodos , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/métodos , Fenómenos Magnéticos , Impresión Molecular/métodos
9.
J Sep Sci ; 45(19): 3735-3744, 2022 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-35932475

RESUMEN

In the current study, a combination of microwave-assisted solvent extraction combined with effervescence-assisted deep eutectic solvent-based in-syringe dispersive liquid-liquid microextraction has been developed as a new sample pretreatment method. The offered method was used for the extraction of five triazine pesticides (atrazine, propazine, cyanazine, ametryn, and simazine) from apple samples before their determination by gas chromatography-flame ionization detection. For this purpose, briefly, the apple sample was contacted with a suitable acidified extraction solvent and the mixture was exposed to microwave irradiations. Then, the supernatant was taken and mixed with a few microliters of a low-density deep eutectic solvent. The supernatant phase containing the extracted analytes was injected into a sodium bicarbonate solution filled into a syringe. Consequently, the effervescence reaction occurs and the analytes were extracted into the fine droplets of extractant dispersed throughout the solution. Afterward, an aliquot of this phase was analyzed by the chromatographic system. Satisfactory outcomes include high enrichment factors (228-261) and extraction recoveries (67-87%), good repeatability (relative standard deviations equal to or less than 3.2% and 5.3% for intra- and inter-day precisions), and low limits of detection (0.4-0.7 ng/g) and quantification (1.4-2.3 ng/g) were acquired under the best experimental situations.


Asunto(s)
Atrazina , Microextracción en Fase Líquida , Malus , Plaguicidas , Microextracción en Fase Líquida/métodos , Plaguicidas/análisis , Solventes/química , Disolventes Eutécticos Profundos , Microondas , Jeringas , Atrazina/análisis , Simazina/análisis , Bicarbonato de Sodio , Triazinas/análisis
10.
J Sep Sci ; 45(14): 2642-2651, 2022 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-35510591

RESUMEN

In this work, iron (III) oxinate magnetic nanocomposite was synthesized and employed as an efficient sorbent for the magnetic dispersive solid-phase extraction of some polycyclic aromatic hydrocarbons from honey samples. In the following, dispersive liquid-liquid microextraction procedure was used for further preconcentration of the analytes. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffractometry, vibrating sample magnetometry, energy dispersive X-ray spectroscopy, and scanning electron microscopy. The results verified the successful formation of the magnetic sorbent. In the extraction process, the sorbent was added into an aqueous solution and the mixture was vortexed. After completing the adsorption process, the supernatant phase was separated in the presence of a magnet and the analytes adsorbed onto sorbent were eluted by acetonitrile. Then, microliter-level 1,1,1-trichloroethane was mixed with the obtained acetonitrile and injected into NaCl solution. Finally, one microliter of the sedimented phase was injected into gas chromatography-flame ionization detector after centrifugation. Under the optimum conditions, a great repeatability (relative standard deviation equal or less than 5 and 6% for intra- and interday precisions, respectively), acceptable extraction recoveries (59-84%), high enrichment factors (118-168), and low limits of detection and quantification (0.16-0.36 and 0.56-1.22 ng/g, respectively) were acquired.


Asunto(s)
Miel , Microextracción en Fase Líquida , Nanocompuestos , Hidrocarburos Policíclicos Aromáticos , Acetonitrilos , Hierro , Límite de Detección , Microextracción en Fase Líquida/métodos , Fenómenos Magnéticos , Hidrocarburos Policíclicos Aromáticos/análisis , Extracción en Fase Sólida/métodos
11.
J Sep Sci ; 45(14): 2652-2662, 2022 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-35596522

RESUMEN

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%).


Asunto(s)
Miel , Microextracción en Fase Líquida , Plaguicidas , Miel/análisis , Microextracción en Fase Líquida/métodos , Plaguicidas/análisis , Poliestirenos , Extracción en Fase Sólida/métodos , Solventes/química
12.
J Sep Sci ; 45(11): 1894-1903, 2022 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-35353940

RESUMEN

A temperature-induced counter-current homogenous liquid-liquid extraction procedure performed in a burette has been proposed for the isolation of aflatoxins B1, B2, G1, and G2 from various fruit chip samples. In this method, a homogenous solution of deionized water and cyclohexylamine is added to the solid sample and the resulted mixture is vortexed. In the following, the liquid phase is taken and passed through the burette filled with a mixture of calcium oxide (as a phase separation agent) and sand (to avoid clumping the calcium oxide). By doing so, the temperature of the solution is increased by hydration of calcium oxide and consequently, the homogenous state is broken and the aflatoxins are migrated into the resulted tiny droplets of cyclohexylamine. This phase is collected on the top of the solution owing to its low density with respect to an aqueous solution. Numerous parameters which can affect the efficiency of the suggested approach were evaluated and under the best situations, great repeatability, low limits of determination and quantification, and high extraction recoveries were acquired. In the end, the suggested approach was employed for the quantification of the selected aflatoxins in various fruit chips samples marketed in Tabriz City, Iran.


Asunto(s)
Aflatoxinas , Aflatoxinas/análisis , Compuestos de Calcio , Cromatografía Líquida de Alta Presión/métodos , Ciclohexilaminas , Frutas/química , Extracción Líquido-Líquido , Óxidos , Espectrometría de Masas en Tándem/métodos , Temperatura
13.
J Sep Sci ; 45(9): 1550-1559, 2022 May.
Artículo en Inglés | MEDLINE | ID: mdl-35220687

RESUMEN

A vortex-assisted dispersive micro-solid-phase extraction procedure using a new and green sorbent was developed as a simple, fast, and efficient sample preparation method for the extracting five pesticides in several fruit juice samples. In this study, for the first time, riboflavin was used as an efficient sorbent. A few milligrams of riboflavin was directly added into the aqueous solution containing the analytes to adsorb them. After adsorption the analytes, they were desorbed and more concentrated by a dispersive liquid-liquid microextraction procedure. The influence of several effective parameters such as amount of riboflavin, pH, vortex time, eluent nature and volume, and extraction solvent type and volume on the extraction efficiency was investigated. In optimal conditions, linear ranges of the calibration curves were broad. The limits of detection and quantification were attained in the ranges of 0.56-1.5  and 1.9-0.52 ng mL-1 , respectively. The proposed method demonstrated to be suitable for concurrent extraction of the studied pesticides in various fruit juice samples with high enrichment factors (320-360) and precision (relative standard deviation ≤7.8% for intra- [n = 6] and interday [n = 4] precisions at a concentration of 25 ng mL-1 of each pesticide).


Asunto(s)
Microextracción en Fase Líquida , Plaguicidas , Jugos de Frutas y Vegetales , Microextracción en Fase Líquida/métodos , Plaguicidas/análisis , Riboflavina , Extracción en Fase Sólida/métodos , Solventes
14.
J Sep Sci ; 45(21): 3974-3984, 2022 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-36106365

RESUMEN

A simple pretreatment method based on the combination of microwave-assisted extraction and dispersive micro solid phase extraction has been developed for the extraction of eprinomectin, doramectin, ivermectin, and abamectin from cow meat, liver, and kidney samples. The extracted drugs were determined using high-performance liquid chromatography equipped with a diode array detector. In this method, the solid samples were mixed with deionized water and organic solvent mixture, and the resulting mixtures were exposed to microwave irradiations to accelerate the analytes' extraction from the samples into the solution. Then, the supernatant was taken and mixed with a mixture of three sorbents optimized by a simplex centroid design. After vortexing and centrifuging, the sorbent particles were isolated and the adsorbed analytes onto the sorbent surface eluted with a natural deep eutectic solvent for more concentration. After centrifuging, the supernatant was taken and injected into the separation system. Acceptable repeatability (relative standard deviations ≤7.0%), high extraction recoveries (72%-86%) and enrichment factors (216-258), and low limits of detection and quantification (0.06-0.10 and 0.19-0.32 ng/g, respectively) were acquired. The method was successfully applied for the assessment of the analytes in the mentioned samples and ivermectin was found in three samples.


Asunto(s)
Microextracción en Fase Líquida , Animales , Bovinos , Microextracción en Fase Líquida/métodos , Microondas , Antiparasitarios , Ivermectina , Extracción en Fase Sólida/métodos , Solventes/química , Carne , Riñón , Hígado
15.
J Sep Sci ; 45(18): 3582-3593, 2022 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-35964286

RESUMEN

A combination of modified quick easy cheap effective rugged and safe extraction approach with carbon nano-onions-based dispersive solid-phase extraction and dispersive liquid-liquid microextraction was developed for the extraction of several pesticides (diazinon, chlorpyrifos, tebuconazole, deltamethrin, permethrin, haloxyfop-methyl, penconazole, and cyhalothrin) from grape before their analysis by gas chromatography-flame ionization detection. In the extraction approach, an aliquot of grape sample is chopped and after separating its juice, the pesticides that remained in the refuse are extracted by the quick, easy, cheap, effective, rugged, and safe extraction method. The obtained acetonitrile phase is mixed with juice and the analytes are extracted by the carbon nano-onions-based dispersive solid-phase extraction. The analytes are concentrated using the microextraction procedure to obtain high enrichment factors. The results showed low limits of detection (0.5-1.6 ng/g) and quantification (1.8-5.4 ng/g) with satisfactory linearity of the calibration curves (determination coefficient, r2 ≥ 0.994). The precision of the developed method expressed as relative standard deviations was good (≤7.2%). The method provided high enrichment factors (350-410) and extraction recoveries (70-82%). Finally, seven grape samples were analyzed successfully.


Asunto(s)
Cloropirifos , Microextracción en Fase Líquida , Plaguicidas , Vitis , Acetonitrilos , Carbono/análisis , Cloropirifos/análisis , Diazinón/análisis , Microextracción en Fase Líquida/métodos , Cebollas , Permetrina/análisis , Plaguicidas/análisis , Extracción en Fase Sólida/métodos
16.
Biomed Chromatogr ; 36(7): e5371, 2022 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-35305038

RESUMEN

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.


Asunto(s)
Espectrometría de Masas en Tándem , Aguas Residuales , Celulosa , Cromatografía Líquida de Alta Presión/métodos , Metoprolol , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos
17.
J Sep Sci ; 44(22): 4167-4180, 2021 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-34558180

RESUMEN

In the present work, a dispersive liquid-liquid microextraction approach has been developed for extraction of four phytosterols (stigmasterol, ß-sitosterol, campesterol, and brassicasterol) from cow milk samples using organic and deep eutectic solvents and the results were critically compared. The extracted analytes were determined using high performance liquid chromatography. In the developed method, carbon tetrachloride and choline chloride:p-chlorophenol deep eutectic solvent were selected to use as the best extraction solvent. Effective parameters and validation data were studied for both methods, independently. Under optimum conditions, limits of detection and quantification were within the ranges of 0.3-0.9 and 1.0-3.0 ng/mL for organic solvent based dispersive liquid-liquid microextraction and 0.09-0.32 and 0.3-1.0 ng/mL for deep eutectic solvent based dispersive liquid-liquid microextraction, respectively. Good coefficient of determinations and relative standard deviations obtained for the methods were ≥0.994 and ≤7.6%, respectively. The introduced method was performed on different milk samples for the determination of target analytes using both solvents and the results were analyzed statistically by the t-test.


Asunto(s)
Leche/química , Fitosteroles/análisis , Animales , Colestadienoles/análisis , Colesterol/análogos & derivados , Colesterol/análisis , Cromatografía Líquida de Alta Presión/métodos , Disolventes Eutécticos Profundos/análisis , Contaminación de Alimentos/análisis , Límite de Detección , Microextracción en Fase Líquida/métodos , Residuos de Plaguicidas/análisis , Solventes/análisis
18.
J Sep Sci ; 44(10): 2121-2130, 2021 May.
Artículo en Inglés | MEDLINE | ID: mdl-33720499

RESUMEN

In this study, a new floating dispersive solid phase extraction method based on deep eutectic solvents has been developed in a home-made extraction device for the extraction of four tetracycline antibiotics from milk samples. In this approach, the sorbent (activated carbon) was dispersed in whole parts of solution with the aid of air stream and floated on top of the solution with the aid of the surfactant (lauryl betaine) and air bubbles. After collection of the sorbent, the adsorbed analytes were eluted with tetrabutyl ammonium chloride-propionic acid deep eutectic solvent under sonication. In this method, there was no need of organic dispersive and extraction solvents and the used sorbent was collected on top of the solution and collected without centrifugation. The validation parameters showed that low limits of detection (0.1-0.3 µg/kg) and quantification (0.6-1.0 µg/kg), acceptable enrichment factors (52-60), efficient extraction recoveries (80-91%), and satisfactory relative standard deviations (≤9.8%) were obtained. Eventually, the method was successfully applied on different milk samples and tetracycline was determined in them.


Asunto(s)
Antibacterianos/aislamiento & purificación , Residuos de Medicamentos/aislamiento & purificación , Leche/química , Extracción en Fase Sólida/métodos , Tetraciclinas/aislamiento & purificación , Adsorción , Animales , Antibacterianos/análisis , Bovinos , Residuos de Medicamentos/análisis , Contaminación de Alimentos/análisis , Límite de Detección , Extracción en Fase Sólida/instrumentación , Solventes , Tensoactivos/química , Tetraciclinas/química
19.
J Sep Sci ; 44(2): 576-584, 2021 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-33151627

RESUMEN

A solid-phase extraction method combined with deep eutectic solvent-based dispersive liquid-liquid microextraction has been developed for the extraction of three antibiotics in honey samples prior to their determination by ion mobility spectrometry. In this method, first, a multiwall carbon nanotube/urea-formaldehyde nanocomposite was synthesized using co-precipitation polymerization method and then it was used as a sorbent for the analytes extraction from the samples. After that the adsorbed analytes were eluted from the sorbent using a water-miscible organic solvent. The collected elution solvent was mixed with tetrabutylammonium chloride:butanol deep eutectic solvent and the mixture was applied in the following microextraction method. The method provided low limits of detection and quantification in the ranges of 0.32-0.86 and 1.1-2.9 ng/g, respectively. The method had a proper repeatability expressed as relative standard deviation less than or equal to 9.1%. The validated method was successfully performed on different honey samples obtained from different producers.


Asunto(s)
Antibacterianos/análisis , Miel/análisis , Microextracción en Fase Líquida , Residuos de Plaguicidas/análisis , Extracción en Fase Sólida , Adsorción , Butanoles/química , Formaldehído/química , Nanotubos de Carbono/química , Tamaño de la Partícula , Compuestos de Amonio Cuaternario/química , Solventes/química , Propiedades de Superficie , Urea/química
20.
J Sep Sci ; 44(7): 1501-1509, 2021 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-33450131

RESUMEN

A new extraction procedure based on combination of a solvent extraction and deep eutectic solvent based dispersive liquid-liquid microextraction has been introduced for the extraction of aflatoxin M1 from cheese samples. In this method, acetonitrile, deionized water, and n-hexane are added onto the sample and vortexed. Owning to different affinities of the substances in cheese toward the mentioned solvents, an efficient and selective extraction of the analyte is done in the acetonitrile phase. After centrifugation, the acetonitrile phase is removed and mixed with a new hydrophobic deep eutectic solvent prepared from N,N-diethanol ammonium chloride and carvacrol as an extraction solvent. The mixture is injected into deionized water, and a cloudy solution is obtained. Eventually, an aliquot of the organic phase is injected into high-performance liquid chromatography-fluorescence detection. After optimizing the effective parameters with the response surface methodology and a quadratic model, limits of detection and quantification were 0.74 and 2.56 ng/kg, respectively. The obtained extraction recovery and enrichment factor were 94% and 94, respectively. Also, intra- (n = 6) and interday (n = 4) precisions were less than or equal to 8.6% at a concentration of 5 ng/kg. The suggested method was applied to determine aflatoxin M1 in different cheese samples.


Asunto(s)
Aflatoxina M1/análisis , Cloruro de Amonio/química , Queso/análisis , Cimenos/química , Etanol/química , Microextracción en Fase Líquida , Solventes/química , Propiedades de Superficie
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