Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 49
Filtrar
1.
Chemosphere ; 335: 139168, 2023 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-37295689

RESUMO

Carbon nanotubes were used to immobilize Chrysosporium fungus for building an adequate adsorbent to be used as an desirable sorbent for preconcentration and measurement of cadmium ultra-trace levels in various samples. After characterization, the potential of Chrysosporium/carbon nanotubes for the sorption of Cd(II) ions was scrutinized by the aid of central composite design, and comprehensive studies of sorption equilibrium, kinetics and thermodynamic aspects were accomplished. Then, the composite was utilized for preconcentration of ultra-trace cadmium levels, by a mini-column packed with Chrysosporium/carbon nanotubes, before its determination with ICP-OES. The outcomes vouchsafed that (i) Chrysosporium/carbon nanotube has a high tendency for selective and rapid sorption of cadmium ion, at pH 6.1, and (ii) kinetic, equilibrium, and thermodynamic studies showed a high affinity of the Chrysosporium/carbon nanotubes for cadmium ion. Also, the outcomes displayed that cadmium can quantitatively be sorbed at a flow speed lesser than 7.0 mL/min and a 1.0 M HCl solution (3.0 mL) was sufficient to desorbe the analyte. Eventually, preconcentration and measurement of Cd(II) in different foods and waters were successfully accomplished with good accuracy, high precision (RSDs ≤5.65%), and low limit of detection (0.015 µg/L).


Assuntos
Chrysosporium , Nanotubos de Carbono , Nanotubos de Carbono/química , Cádmio/química , Adsorção , Indicadores e Reagentes , Íons , Concentração de Íons de Hidrogênio , Espectrofotometria Atômica
2.
Environ Sci Pollut Res Int ; 30(2): 3121-3132, 2023 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-35945321

RESUMO

Keeping selectiveness and efficiency in view with solid-phase microextraction (SPME) of metal ions, this work was aimed at synthesis of a novel modified sorbent on a stainless-steel surface to fabricate a selective and efficient fiber for SPME of mercury ions from real food and biological samples. After the confirmation of sorbent structure grafted on the stainless-steel surface, by different techniques, the synthesized fiber was utilized for extraction and preconcentration of mercury before its measurement by an inductively coupled plasma-optical emission spectroscopy (ICP-OES). For optimizing the efficiency, the influences of various factors on the extraction of Hg (II) ion were scrutinized. The optimized values used for extraction were pH 7.0, adsorption time 8 min, desorption time 5 min, 5 mL of eluent solvent containing nitric acid with concentration of 0.5 mol L-1, and stirring rate of 300 rpm. Underneath optimum condition, the relative standard deviation for 30 extractions, done by one synthesized fiber, was calculated to be 2.89% and for five extractions, done by 5 synthesized fibers, was calculated to be 1.78%. The high performance of the synthesized fiber was checked with high recoveries obtained from 30 successive sorption-desorption cycles, using a unique synthesized fiber. Finally, the suggested procedure was triumphally exploited for extraction and pre-concentration of Hg (II) ion in real food and biological samples.


Assuntos
Mercúrio , Microextração em Fase Sólida , Microextração em Fase Sólida/métodos , Aço Inoxidável/química , Metais/química
3.
Chemosphere ; 308(Pt 2): 136323, 2022 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-36084832

RESUMO

Polyvinyl alcohol (PVA) and sodium alginate (SA) hydrogel-coated nanofiltration (NF) membranes with high-flux and permselectivity were prepared. The coating of PVA and SA hydrogel selective layer on a porous polysulfone (PSf)/non-woven fabric ultrafiltration substrate membrane was conducted through different three procedures including pre-crosslinking, in-situ crosslinking, and immersing crosslinking and the use of glutaraldehyde as a crosslinking agent. The properties and performances of all types of the prepared membranes were evaluated through ATR-FTIR spectroscopy, AFM, SEM, zeta potential, contact angle, and cross-flow permeation tests. The immersing technique resulted in the formation of TFC membranes with higher hydrophilicity, smoother surface layer, higher negative charge, higher permeation flux, higher salt rejection and better anti-fouling performance. Also, the higher negative surface charge of the immersing coated TFC membranes due to dissociation of hydrophilic functional groups of the PVA and SA hydrogel selective layer resulted in higher As(III) rejection. SA coated NF membrane through immersing method exhibited a higher pure water permeability of 11.2 L m-2 h-1 bar-1, NaCl, MgSO4, and Na2SO4 rejection of 38.2%, 55.1%, and 70.4%, respectively with As(III) rejection of 60.6%. All types of the PVA and SA hydrogel-coated PSf membranes possessed improved fouling resistance to BSA aqueous solution, superior anti-fouling performance was obtained with SA hydrogel coating through immersing method. Such optimum membranes indicated high stability in the long-term experiments. This study showed that the coating of the SA hydrogel layer on a PSf support through immersing method could be a promising candidate for fabricating high-flux NF membranes.


Assuntos
Alginatos , Álcool de Polivinil , Alginatos/química , Glutaral , Hidrogéis , Membranas Artificiais , Polímeros , Álcool de Polivinil/química , Cloreto de Sódio , Sulfonas , Água
4.
Mol Divers ; 26(1): 97-112, 2022 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-33387185

RESUMO

Synthesizing new chemical compounds and studying their biological applications have been important issues in scientific research. In this investigation, we synthesized and characterized ten new N-acetyl phosphoramidate compounds and explored the crystal structure of three others. Furthermore, not only were some kinetic inhibition parameters measured, like IC50, Ki, kp, KD for 7 compounds on human acetylcholinesterase (AChE) and butyrylcholinesterase (BChE), but also their hydrophobic parameter was determined by shake-flask technique. All compounds (number 1-10) were investigated for anti-bacterial activity against three Gram-positive and three Gram-negative bacteria, while chloramphenicol was used as a standard antibiotic. In order to find new insecticide, toxicities of 13 acephate (Ace)-derived compounds (number 20-32) were bioassayed on third larval instar of elm leaf beetle and Xanthogaleruca luteola. Additionally, screening in vivo tests revealed that two compounds had had the greatest insecticidal potential in comparison with others. It means these ones inhibited AChE (with mixed mechanisms) and general esterase more than the rest. According to ChE-QSAR models, the inhibitory potency for enzyme and bacteria is directly influenced by the electronic parameters versus structural descriptors. AChE-QSPR model of fluorescence assay indicated that the inhibitory power of AChE is primarily influenced by a set of electronic factors with the priority of: EHB > PL > δ(31P) versus structural descriptor (SA and Mv). Synthesizing new chemical compounds and studying their biological applications have been important issues in scientific research. Toxicities of 13 acephate (Ace)-derived compounds (number 20-32) were bioassayed on third larval instar of elm leaf beetle and Xanthogaleruca luteola. Insect-QSAR equations of these compounds, based on MLR and PCA, showed that non-descriptor net charge nitrogen atom (which was affected by the polarization of N-H group) had the greatest effect on insecticidal potential.


Assuntos
Acetilcolinesterase , Inseticidas , Acetilcolinesterase/metabolismo , Butirilcolinesterase/química , Inibidores da Colinesterase/química , Humanos , Inseticidas/química , Inseticidas/farmacologia , Simulação de Acoplamento Molecular , Relação Estrutura-Atividade
5.
Chemosphere ; 289: 133060, 2022 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-34838830

RESUMO

Epirubicin (EP) and topotecan (TP) are two major anti-cancer compounds for the treatment of breast cancer with serious side effects. Hence herein, a carbon paste electrode (CPE) amplified with Pt/SWCNT nanocomposite and a deep eutectic solvent (CPE/DES/Pt-SWCNT) were proposed as an analytical tool for the monitoring of EP in the presence of TP in the real samples. Amplification of sensor was improve EP oxidation signal about 2.73 times. Under the optimized conditions, EP determined by using differential pulse voltammetry (DPV) technique with linear dynamic range of 0.001-500 µM with limit of detection (LOD) of 0.8 nM. The CPE/DES/Pt-SWCNT offered influential ability for monitoring of EP in injection and dextrose saline samples with a recovery range of 97.4%-104.9%.


Assuntos
Nanocompostos , Topotecan , Carbono , Solventes Eutéticos Profundos , Técnicas Eletroquímicas , Eletrodos , Epirubicina , Solventes
6.
J Educ Health Promot ; 10: 145, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34222520

RESUMO

BACKGROUND: Most patients with myocardial infarction (MI) suffer from one or more risk factors such as obesity and overweight, unhealthy diet, lack of physical activity (PA), and high blood pressure. Individual control of these risk factors by lifestyle modification raises the probability of survival in these patients; hence, we used a self-management intervention to assess its effect on the lifestyle of post-MI patients. MATERIALS AND METHODS: This quasi-experimental study was conducted on 92 hospitalized MI patients in Hamadan province in 2016. Convenience sampling method was used for selecting the participants. The patients were selected and assigned to experimental and control groups. The main parameters (diet, blood pressure, waist circumference, and body mass index [BMI]) were measured at the baseline and 8 weeks after discharge. Domestic PA was the only parameter measured 8 weeks after their discharge. A self-management intervention was adopted for the experimental group. The data were analyzed using paired and independent-sample t-tests with SPSS software version 16. RESULTS: The comparison of the scores obtained for diet, blood pressure, waist circumference, and BMI in post-MI patients revealed no statistically significant difference between the two groups at the beginning of the study (P > 0.05). Following the intervention, the experimental group had a significantly higher mean score for diet and domestic PA (walking program from 1st week to 8 weeks), compared to the control group (P < 0.001); however, the intervention had no significant effect on BMI, waist circumference, and systolic and diastolic pressure (P > 0.05). CONCLUSION: The findings indicated that the program had an impact on some risk factors. Therefore, it is recommended to use self-management support in MI patients during the discharge process to improve their lifestyle.

7.
J Environ Manage ; 294: 112918, 2021 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-34139646

RESUMO

In the present study chitosan-aminopropylsilane graphene oxide (CS-APSGO) nanocomposite hydrogel was synthesized and utilized as a hydrophilic additive in different dosages (0.5, 1, 2 and 5 wt%) in fabrication of porous polyethersulfone (PES) membranes via the phase inversion induced process by immersion precipitation method for heavy metal ion and dye removal. The modified membranes were characterized using ATR-FTIR, AFM, SEM, water contact angle, overall porosity and mean pore radius evaluations and zeta potential measurement. The addition of CS-APSGO nanocomposite hydrogel to PES doping solutions enhanced membranes hydrophilicity and consequently pure water flux permeability. Filtration performance of the CS-APSGO embedded membranes showed promising antifouling properties during BSA filtration test (FRR> 90%) and 1 wt% membranes showed the highest pure water flux of 123.8 L/m2 h with BSA rejection more than 98% and removal capability more than 82% for lead (II) ion, 90.5% and 98.5% for C.I. Reactive Blue 50 and C.I. Reactive Green 19, respectively. Therefore, the CS-APSGO nanocomposite hydrogel blending in order to modification of PES-based membranes have a noticeable potential in improving filtration performance of blended membranes.


Assuntos
Quitosana , Grafite , Chumbo , Membranas Artificiais , Nanogéis , Polímeros , Silanos , Sulfonas
8.
Anal Methods ; 12(18): 2338-2346, 2020 05 14.
Artigo em Inglês | MEDLINE | ID: mdl-32930259

RESUMO

Nanomagnetic graphene oxide modified with dopamine (GO-Fe3O4-DA) was synthesized via a very simple procedure. Using GO-Fe3O4-DA as the new adsorbent, the effervescence-assisted dispersive micro solid-phase extraction procedure was exploited for the preconcentrative extraction of Cu(ii), Pb(ii) and Ni(ii) ions. Structural characteristics of the adsorbent were studied via FT-IR, FE-SEM, EDX and XRD analyses. The rapid dispersion and high adsorption capability of GO-Fe3O4-DA, along with the rapid separation of the adsorbent from the aqueous phase by a magnet, led to a decrease in the extraction time of the target metal ions. In effect, high extraction percentages were attained in a very short time period. In this work, the relative standard deviations (RSD; n = 3) calculated for the proposed method were 1.09, 1.25 and 1.03% for the Pb(ii), Cu(ii) and Ni(ii) ions, respectively, the calibration curve was dynamically linear in the range of 0.25 to 50 µg L-1, and the limits of detection were obtained as 0.5, 0.1, and 0.7 µg L-1. The procedure was also implemented on real sausage (herbal and meaty) samples and a water sample, vouchsafing the success of the proposed method in tackling real samples with a complicated matrix.


Assuntos
Técnicas de Química Analítica , Dopamina , Grafite , Metais , Extração em Fase Sólida , Dopamina/química , Grafite/química , Fenômenos Magnéticos , Metais/isolamento & purificação , Espectroscopia de Infravermelho com Transformada de Fourier
9.
Anal Methods ; 12(40): 4867-4877, 2020 10 22.
Artigo em Inglês | MEDLINE | ID: mdl-32974629

RESUMO

In this paper, a CO2-effervescence assisted dispersive micro solid-phase extraction procedure (CO2-EA-DµSPE) using a magnetic layered double hydroxide modified with polyaniline and a surfactant (Zn-Al-LDH-PA-DBSNa-Fe3O4) was applied for the pre-concentration of heavy metals (Ni2+, Pb2+, Co2+, and Cd2+). The final analysis of the analytes was carried out by atomic absorption spectroscopy. XRD, FTIR, and SEM studies were used for the characterization of the synthesized nanoadsorbent. For the maximum extraction efficiency, effective factors (including pH, nanoadsorbent dosage, and volume of the eluent) were investigated using the central composite design (CCD) method. Under the optimum conditions, the preconcentration factor was more than 20. The linear ranges for Ni2+, Pb2+, Co2+, and Cd2+ were obtained as (5-550), (7-750), (5-500), and (3-100) ng mL-1, respectively. The proposed method provided low detection limits (1.4, 2.1, 1.5, and 0.9 ng mL-1 for Ni2+, Pb2+, Co2+, and Cd2+, respectively) and suitable repeatability (relative standard deviation values (RSDs) below 6.1%, n = 6). Finally, the current method was successfully used for the extraction of heavy metals from cosmetic samples.

10.
Indian J Anaesth ; 64(5): 369-374, 2020 May.
Artigo em Inglês | MEDLINE | ID: mdl-32724244

RESUMO

BACKGROUND AND AIMS: Systemic lignocaine has been shown to have sedative effects. We designed this randomised-double-blind, placebo-controlled study to evaluate the effect of intravenous lignocaine on the bispectral index (BIS) during caesarean section under spinal anaesthesia. METHODS: 80 patients scheduled for elective caesarean section under spinal anaesthesia were randomly allocated to 2 study groups. Group L received intravenous 1.5 mg/kg of lignocaine bolus, 15 minutes before spinal anaesthesia followed by an intravenous infusion 1.5 mg/kg/h for 60 minutes intravenously. The patients in the control group (C group) were given 0.9% sodium chloride in a double-blind fashion. Spinal anaesthesia was performed with 10 mg of 0.5% bupivacaine. The changes of Sao2, BIS and hemodynamic variables during caesarean section, Apgar score of neonate and the incidence of adverse effects were recorded. RESULTS: BIS values were lower in the L group compared to C group (P ≤ 0.001). Comparison of mean arterial pressure (MAP) changes during spinal anaesthesia and surgery reveal statistically significant difference between two groups through repeated measure analysis (P ≤ 0.001), but comparision of heart rate (HR) changes during spinal anaesthesia and surgery failed to reveal any statistically significant difference between two groups. (P = 0.261). The Apgar scores did not reveal a significant difference between the two groups at first and five minutes after delivery (P = 0.99). CONCLUSION: Intravenous lignocaine infusion given with spinal anaesthesia in women undergoing elective caesarean delivery providing lower BIS values without respiratory depression, in the absence of foetal compromise.

11.
Artigo em Inglês | MEDLINE | ID: mdl-31491695

RESUMO

In this work, an efficient method termed as continuous flow membrane microextraction coupled with high performance liquid chromatography is introduced for a highly selective determination of metoprolol and propranolol in the biological samples. According to this method, an aqueous source phase of the analytes (donor phase, 10 mL) is circulated into an extraction cell, which is separated from an aqueous acceptor phase (100 µL) by a small piece of polypropylene membrane sheet whose pores are impregnated by an organic solvent (1-octanol, 15 µL). The analytes are extracted from the donor phase into the organic solvent. They are subsequently selectively back-extracted into the acceptor solution due to the pH gradient. The proposed method is very convenient and has the capability of being fully automated. It provides a good preconcentration and an excellent repeatability. The extractant is an aqueous phase, and by prevention of the extraction of macromolecules through the membrane, the developed method provides a high sample clean-up. In order to maximize the extraction efficiency, the influential parameters including the type of mediator solvent, pH values for the donor and acceptor solutions, extraction time, ionic strength, stirring rate, and volume of the acceptor solution are optimized. The calibration curves were obtained with a reasonable linearity (r2 = 0.999) in the range of 3-1000 ng mL-1. The limits of detection were 0.5 and 1.0 ng mL-1, and excellent relative standard deviations were obtained (between 3.2% and 4.0%). Finally, the reliability of the procedure is evaluated by determination of metoprolol and propranolol in the human urine and plasma samples, which indicates the suitability, sensitivity, and high sample clean-up of the proposed method.


Assuntos
Antagonistas Adrenérgicos beta/sangue , Antagonistas Adrenérgicos beta/urina , Cromatografia Líquida de Alta Pressão/métodos , Microextração em Fase Líquida/métodos , Antagonistas Adrenérgicos beta/química , Antagonistas Adrenérgicos beta/isolamento & purificação , Desenho de Equipamento , Humanos , Limite de Detecção , Modelos Lineares , Microextração em Fase Líquida/instrumentação , Reprodutibilidade dos Testes
12.
J Chromatogr A ; 1608: 460409, 2019 Dec 20.
Artigo em Inglês | MEDLINE | ID: mdl-31399210

RESUMO

In this study two different analytical approaches have been developed to determine the presence of several cyanotoxins in saline water samples from a continental salt marsh. A salting-out assisted liquid-liquid extraction (SALLE) has been used in combination with ultra-high performance liquid chromatography-tandem mass spectrometry and UV-diode array detection (UHPLC-MS/MS and UHPLC-DAD). The target analytes are eight microcystins named MC-RR, MC-YR, MC-LR, MC-WR, MC-LA, MC-LY, MC-LW, MC-LF and nodularin (NOD), covering a wide range of polarities. The separation was achieved using a Zorbax Eclipse Plus RRHD C18 column (50 × 2.1 mm, 1.8 µm) in less than 7.5 and 5.5 min for UV and MS/MS detection, respectively. The mobile phase used consisted of water (solvent A) and acetonitrile (MeCN) (solvent B), both containing 0.01% of formic acid for DAD and 0.4% of formic acid for MS/MS detection, at a flow rate of 0.4 mL min-1. The temperature of the column was set at 25 °C and 20 µL of sample were injected. The main parameters affecting the SALLE procedure were studied and the following optimum values were obtained: neutral pH, 2 mL of acetonitrile as extraction solvent and 1.2 g of ammonium sulfate as salting-out agent for 4 mL of water sample. The validation protocols for both methods were accomplished with real water samples obtaining LODs ranging from 1.0 to 3.4 µg L-1 and 0.02 to 0.11 µg L-1 for DAD and MS/MS respectively. Although the SALLE-UHPLC-DAD methodology is easier and cheaper than UHPLC-MS/MS significantly better detection limits were achieved with tandem mass spectrometry as well as allowing for unambiguous identification. Extraction recoveries were higher than 77.0% (except for MC-RR and NOD which were 53.2% and 54.3, respectively) with satisfactory inter-day and intra-day precisions (RSD below 13.3%).


Assuntos
Cromatografia Líquida de Alta Pressão , Monitoramento Ambiental/métodos , Extração Líquido-Líquido , Toxinas Marinhas , Microalgas/química , Água do Mar/química , Espectrometria de Massas em Tandem , Limite de Detecção , Toxinas Marinhas/análise , Toxinas Marinhas/isolamento & purificação , Microcistinas/análise , Microcistinas/isolamento & purificação , Reprodutibilidade dos Testes , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação
13.
Food Chem ; 286: 185-190, 2019 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-30827594

RESUMO

An in-situ chemical reaction based dispersive procedure termed as CO2-effervescence assisted emulsification microextraction was first utilized for pre-concentration of Sudan dyes in spices. It is simple, quick, and efficient; based on a switchable fatty acid (hexanoic acid, pKa ∼ 4.8). The extraction agent is able to be switched into hydrophobic/hydrophilic forms in pH-changeable media, leading to facile and effective dispersion and phase's separation. The method was proved by the analysis of spiked samples. Optimization was statistically performed, resulted in maximum extraction efficiencies. Under optimal conditions, method validation was assayed in the aqueous solutions. Wide linearity with high R2 values and low detection limits (1-5 ng mL-1) were obtainable. Also, enrichment factors were 62-66 with proper repeatability (%RSDs < 6.8, n = 3). Good validations in terms of recovery (86.6-104.5%) and repeatability (%RSDs < 7.8, n = 3, C = 15 and 30 µg g-1) in foodstuffs confirmed a great effectiveness of the method in complex matrices.


Assuntos
Compostos Azo/análise , Cromatografia Líquida de Alta Pressão/métodos , Análise de Alimentos/métodos , Microextração em Fase Líquida/métodos , Especiarias/análise , Dióxido de Carbono/química , Emulsões/química , Ácidos Graxos/química , Contaminação de Alimentos/análise , Concentração de Íons de Hidrogênio , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Reprodutibilidade dos Testes , Solventes/química
14.
Artigo em Inglês | MEDLINE | ID: mdl-30522049

RESUMO

For the first time, three phase hollow fiber liquid phase microextraction using an influential, and green middle phase comprised a new relatively-hydrophobic deep eutectic solvent (three-phase HF-LPME-DES) was developed for trace analyses of antiarrhythmic drugs in biological and environmental samples. The extraction solvent was easily synthesized by mixing the green and cheap raw materials, namely choline chloride and 1-phenylethanol (ChCl: Ph-ETOH), in the ambient temperature. Good compatibility to pores of hollow-fiber, high ability for extraction of ionizable organic compounds with no need to any carrier agents, and easy availability in the laboratory environment turned this new proposed deep eutectic intermediate to a worthy generation of the supported liquid membrane (SLM). Final determination was accurately done by high performance liquid chromatography-ultraviolet detection (HPLC-UV). After effective statistical optimization of main parameters, the valid analytical features were found to be: wide linear dynamic ranges (LDRs) of 0.8 to 500 ng mL-1 with the determination coefficients (R2s) higher than 0.98, low detection limits (LODs) of 0.3-0.8 ng mL-1, and logical precision (relative standard deviations (%RSDs, n = 3) of 5.2-6.5%). Also, enrichment factors and extraction recoveries were 110-135 and 44-54%, respectively. These satisfactory results confirmed the potent effectiveness of the proposed microextraction procedure for achievement to clean and proper enrichment of the aforesaid compounds in highly complex real samples.


Assuntos
Antiarrítmicos/isolamento & purificação , Microextração em Fase Líquida/métodos , Antiarrítmicos/análise , Álcoois Benzílicos , Colina , Cromatografia Líquida de Alta Pressão , Química Verde , Humanos , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes
15.
Anal Chim Acta ; 1047: 275-284, 2019 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-30567660

RESUMO

In this work, a rapid and simple method is applied using a newly synthesized nanoadsorbent for the extraction and preconcentration of the drugs Amitriptyline (AMT) and Nortriptyline (NRT), which are then determined using high performance liquid chromatography. We focus on the facile synthesis of Fe3O4@SiO2@N3, as a new and effective adsorbent, and the effervescent salt-assisted dispersive magnetic micro solid-phase extraction method. The applied method and modification of the surface of Fe3O4@SiO2 with the nitrogen-rich group lead to an increase in the interaction between the nanoadsorbent used and the analytes, and increase the extraction recovery. The accuracy of the synthesized nanoadsorbent is confirmed by the FT-IR, FE-SEM, XRD, and VSM analytical techniques. In order to obtain the best experimental conditions, optimization of the main variables involved is carried out using the central composite design method. Under the optimum experimental conditions, the limits of detection (LODs), linear dynamic ranges (LDRs), and relative standard deviations (RSDs for n = 5) for NRT and AMT were found to be as follow: LODs, 0.03 and 0.05 ng/mL; RSDs, 2.04 and 1.1 for NRT and AMT, respectively; and LDRs, 0.07-2000 ng/mL. Furthermore, the results obtained show that the nanoadsorbent can be used for five times with an extraction recovery more than 80% and 70% for AMT and NRT, respectively.


Assuntos
Amitriptilina/análise , Azidas/química , Nanopartículas de Magnetita/química , Nortriptilina/análise , Dióxido de Silício/química , Adsorção , Amitriptilina/química , Humanos , Limite de Detecção , Nortriptilina/química , Microextração em Fase Sólida/métodos , Águas Residuárias/análise
16.
J Chromatogr A ; 1576: 1-9, 2018 Nov 16.
Artigo em Inglês | MEDLINE | ID: mdl-30314683

RESUMO

In this study, a new extraction medium based on a quite bio-compatible and bio-degradable deep eutectic solvent comprising choline chloride and phenylethanol (ChCl: Ph-ETOH) was simply and cheaply synthesized at room temperature. At the next step, it was effectively utilized at the service of air agitated-emulsification microextraction (AA-EME) of two major amphetamine-type stimulants (ATSs) in human plasma and pharmaceutical wastewater pursued by high performance liquid chromatography-ultraviolet detection (HPLC-UV). This safe, effective, and rapid enrichment process based on the new low-density DES was easily practicable via a homemade extraction cell possessing a narrow neck and with no extra demand the emulsifier intermediates. Statistical study of main parameters effects using central composite design (CCD) combined with desirability function (DF) demonstrated that pH 12, 250 µL of extraction solvent, 8 air agitation cycles, and 5% of salt amount resulted in maximum extraction efficiencies (63-66%) with DF value close to 0.98. Under optimal conditions, wide linear dynamic ranges (LDRs) of 15.0-2000 and 8.0-3000 ng mL-1 with the determination coefficients (R2s) close to 0.99 were obtainable for amphetamine and methamphetamine, respectively. Low limits of detection (LODs) as well as relative standard deviations (%RSDs, n = 3) were found to be 2.0-5.0 ng mL-1 and 5.7-7.8%, respectively. Also, enrichment factors (EFs) were quantitative in the span of 47-50. On the other hand, satisfactory and accurate assessment at low levels close to therapeutic and toxic domains in human plasma sample and pharmaceutical wastewater was successfully obtained.


Assuntos
Anfetamina/isolamento & purificação , Análise Química do Sangue/métodos , Microextração em Fase Líquida/métodos , Metanfetamina/isolamento & purificação , Solventes/química , Águas Residuárias/química , Análise Química do Sangue/economia , Cromatografia Líquida de Alta Pressão , Humanos , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Microextração em Fase Líquida/economia
17.
J Sep Sci ; 41(15): 3097-3104, 2018 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-29943450

RESUMO

In this work, an efficient microextraction method was applied for the extraction of some chlorophenols in water samples. This method, termed filter-based emulsification microextraction, is based on the dispersion of an extractant into an aqueous sample solution to accelerate the extraction process and the utilization of a Nylon syringe filter to break the emulsion. After phase separation, the method is coupled with gas chromatography as a final analyzer instrument. The overall derivatization/extraction time was about 90 s. The proposed method is centrifuge-free, and it also provides a suitable sample clean-up by filtration of the extracting phase. The effective parameters involved in the extraction method were optimized. Under the optimal experimental conditions, the method provided a good linearity in the range of 2.0-2000 ng/mL, extraction repeatabilities (relative standard deviations) below 9.4%, enrichment factors of 180-203, and limits of detection between 0.5 and 1.2 ng/mL.

18.
Electron Physician ; 10(4): 6624-6630, 2018 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-29881524

RESUMO

BACKGROUND: Open heart surgery is one of the most common and valuable treatment methods for cardiovascular diseases, a common side effect of which is atrial fibrillation that occurs due to various reasons. OBJECTIVE: To determine the relationship between incidence of atrial fibrillation (AF) and duration of cardiopulmonary bypass (CPB) in patients after open heart surgery. METHODS: The present retrospective cohort study was conducted on 330 patients in Farshchian Heart Center through census. The required data were collected from medical records of the patients undergoing coronary bypass surgery using data collection between April 2015 and March 2015. Then, data analysis was performed using SPSS software (ver.16) at error level of p<0.05. The tests used in this study included independent-samples t-test, Mann-Whitney, and chi-squared tests. RESULTS: Based on the results, mean age of the patients was 61.76±9.2, the majority of the patients (70.1%) were male. The association between Incidence of Atrial Fibrillation and cardiopulmonary pump time (minute) was not meaningful. Incidence of atrial fibrillation had statistically significant relationship with variables of mean age, BMI, PAC, PVC, creatinine and duration of hospitalization (p<0.05); on the other hand, variables of gender, cross clamp time (minute), intubation time (hour), and clinical history had no effect on atrial fibrillation incidence rate (p>0.05). CONCLUSION: Since the pathogenesis of AF after cardiac surgery is believed to be multifactorial, including clinical variables and technical intraoperative factors, the relation between incidence of AF with mean age, BMI, PAC, PVC, creatinine and duration of hospitalization was significant. But AF was not related to cardiopulmonary pump time (minute). It is necessary to conduct further research on factors affecting incidence of atrial fibrillation.

19.
Mikrochim Acta ; 185(3): 160, 2018 02 06.
Artigo em Inglês | MEDLINE | ID: mdl-29594695

RESUMO

This review (with 151 refs) focuses on recent progress that has been made in magnetic nanoparticle-based solid phase extraction (SPE), pre-concentration and speciation of heavy metal ions. In addition, it discusses applications to complex real samples such as environmental, food, and biological matrices. The introduction addresses current obstacles and limitations associated with established SPE approaches and discusses the present state of the art in different formats of off-line and on-line SPE. The next section covers magnetized inorganic nanomaterials for use in SPE, with subsections on magnetic silica, magnetic alumina and titania, and on magnetic layered double oxides. A further section treats magnetized carbonaceous nanomaterials for use in SPE, with subsections on magnetic graphene and/or graphene oxides, magnetic carbon nanotubes and magnetic carbon nitrides. We then discuss the progress made in SPE based on the use of magnetized organic polymers (mainly non-imprinted and ion-imprinted polymer). This is followed by shorter sections on the use of magnetized metal organic frameworks, magnetized ionic liquids and magnetized biosorbents. All sections include discussions of the nanomaterials in terms of selectivity, sorption capacity, mechanisms of sorption and common routes for material synthesis. A concluding section addresses actual challenges and discusses perspective routes towards further improvements. Graphical abstract An overview on booster nanomaterials (ionic liquids, inorganic, organic and biological materials, and metal-organic frameworks) for use in magnetic nanoparticle-based solid-phase extraction of heavy metal ions.

20.
J Sep Sci ; 41(10): 2214-2220, 2018 May.
Artigo em Inglês | MEDLINE | ID: mdl-29427354

RESUMO

In this work, a simple method, namely, tandem dispersive liquid-liquid microextraction, with a high sample clean-up is applied for the rapid determination of the antidementia drugs rivastigmine and donepezil in wastewater and human plasma samples. This method, which is based on two consecutive dispersive microextractions, is performed in 7 min. In the method, using a fast back-extraction step, the applicability of the dispersive microextraction methods in complicated matrixes is conveniently improved. This step can be performed in less than 2 min, and very simple tools are required for this purpose. To achieve the best extraction efficiency, optimization of the variables affecting the method was carried out. Under the optimized experimental conditions, the relative standard deviations for the method were in the range of 6.9-8.7%. The calibration curves were obtained in the range of 2-1100 ng/mL with good correlation coefficients, higher than 0.995, and the limits of detection ranged between 0.5 and 1.0 ng/mL.


Assuntos
Inibidores da Colinesterase/análise , Indanos/análise , Fármacos Neuroprotetores/análise , Piperidinas/análise , Rivastigmina/análise , Águas Residuárias/química , Algoritmos , Calibragem , Inibidores da Colinesterase/sangue , Cromatografia Líquida de Alta Pressão , Donepezila , Humanos , Concentração de Íons de Hidrogênio , Indanos/sangue , Limite de Detecção , Modelos Lineares , Microextração em Fase Líquida , Fármacos Neuroprotetores/sangue , Piperidinas/sangue , Plasma/química , Reprodutibilidade dos Testes , Rivastigmina/sangue , Sais , Solventes
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA