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1.
J Dent (Shiraz) ; 25(2): 147-154, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38962084

RESUMO

Statement of the Problem: Successful endodontic treatment depends on three-dimensional (3D) root canal filling to prevent the leakage of residual bacteria. Different obturation techniques with different sealers should be compared by employing advanced assessment tools. Purpose: This study compared the obturation quality of warm vertical compaction (WVC) and two different single-cone (SC) techniques using micro-computed tomography (micro-CT). Materials and Method: Thirty-three extracted maxillary molars with mesial root canal curvature of 20‒40º were prepared in vitro with One-Curve files and randomly assigned to three groups (n=11) for root canal obturation with WVC, SC technique with AH Plus sealer (SC-AH), or SC technique with SureSeal bioceramic (BC) sealer (SC-Su). The root canals underwent micro-CT examinations before and after obturation to determine the volume percentages (VPs) of voids and gaps at different distances from the apex (coronal, middle, and apical thirds). Data were analyzed by Kruskal-Wallis and Mann-Whitney U tests. Results: The highest VP of voids and gaps was recorded in the SC-Su group, with no significant difference from other groups (p> 0.05). There were significant differences in VP of gaps at different distances from the apex (p<0.05). The VPs of gaps in the apical third of all the samples were significantly higher than in the coronal and middle thirds. However, the difference in VP of voids was not significant at different distances from the apex (p>0.05). Conclusion: None of the tested techniques could provide a void-free and gap-free filling. The apical third of the canals showed the highest VP of gaps in all obturation techniques.

2.
Sci Rep ; 14(1): 9129, 2024 Apr 21.
Artigo em Inglês | MEDLINE | ID: mdl-38644395

RESUMO

Graphene allotropes with varied carbon configurations have attracted significant attention for their unique properties and chemical activities. This study introduces a novel two-dimensional carbon-based material, termed Graphsene (GrS), through theoretical study. Comprising tetra-, penta-, and dodeca-carbon rings, GrS's cohesive energy calculations demonstrate its superior structural stability over existing graphene allotropes, including graphyne and graphdiyne families. Phonon dispersion analysis confirms GrS's dynamic stability and its relatively low thermal conductivity. All calculated GrS elastic constants meet the Born criteria, ensuring mechanical stability. Ab-initio molecular dynamic simulations show GrS maintains its structure at 300 K. HSE06 calculations reveal a narrow electronic bandgap of 20 meV, with the electronic band structure featuring a highly anisotropic Dirac-like cone due to its intrinsic structural anisotropy along armchair and zigzag directions. Notably, GrS is predicted to offer exceptional catalytic performance for the oxygen reduction reaction, favoring the four-electron reduction pathway with high selectivity under both acidic and alkaline conditions. This discovery opens promising avenues for developing metal-free catalyst materials in clean energy production.

3.
Food Chem ; 410: 135383, 2023 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-36638629

RESUMO

A nanosensor is designed for rapid detection of the gluten content of wheat-containing samples. Gluten is a plant protein that causes allergy in individuals and leads to celiac disease. Since in a celiac diet trace amounts of gluten are able to prompt allergic reactions, a food-allergen label must be provided on foodstuffs and be seriously considered by food industries. Various analytical methods and commercial immunoassays are used for such analyses but prices per test, especially for low-income countries are high. Thus, a rapid, sensitive, simple, and inexpensive detecting tool seems essential. A solution can be designing a gluten optical nanosensor. The nanosensor is made of folic-acid-carbon dots and gluten molecularly templates embedded simultaneously in a silicate matrix. Adding gluten to the solution of this nanostructure and its adsorbing on the blank templated space on the nanostructure causes fluorescence enhancement. The concentration range of gluten detection was 0.36 to 2.20 µM.


Assuntos
Doença Celíaca , Hipersensibilidade Alimentar , Humanos , Glutens/análise , Carbono/química , Triticum , Dieta , Corantes Fluorescentes/química
4.
Iran Endod J ; 17(3): 114-120, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-36704085

RESUMO

Introduction: Pain management during root canal therapy and after that is of great importance in endodontics. This study aimed to compare the effect of two non-steroidal anti-inflammatory drugs (NSAIDs); ibuprofen and ibuprofen lysine with two methods of prescription on pain after single-visit root canal treatment of first and second mandibular molar teeth with irreversible pulpitis. Materials and Methods: This randomized study recruited subjects experiencing moderate to severe pain from a tooth diagnosed with symptomatic irreversible pulpitis (n=120). Subjects were randomized to receive 400 mg ibuprofen acid or 400 mg ibuprofen lysine regularly or on demand. The primary objective was to measure changes in pain scores at post-operative time frames of 6, 12, 18, 24, 48 and 72 hours after the root canal treatment on a 0-10 numerical rating scale (NRS). Independent T-test, Non-parametric Kruskal-Wallis Test and Friedman Test were used to analyze the data. Results: Kruskal-Wallis analysis showed a significant difference in NRS score between on-demand ibuprofen group and regular ibuprofen group and also between regular ibuprofen lysine group and regular ibuprofen group at 6 hours after the treatment (P<0.05). But no remarkable difference was observed in the recorded mean pain intensity of four study groups in the other time frames (P>0.05). Conclusions: Based on this randomized clinical trial, there was no significant difference in the pain intensity of patients using ibuprofen and ibuprofen lysine. Additionally, there was no significant difference in the degree of pain between the on-demand and regular groups, despite the fact that patients in the on-demand group used less medications. Due to the multiple negative effects of NSAIDs, it would be wise to prescribe ibuprofen on demand.

5.
J Chromatogr A ; 1627: 461413, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823111

RESUMO

Innovations in extraction phases, extraction modes and hyphenated instrument configurations, are the most important issues to address for progress in the solid phase microextraction (SPME) methodology. In this regard, we have embarked on the development of a novel biocompatible 96-monolithic inorganic hollow fiber (96-MIHF) array as a new configuration for high-throughput SPME on a 96-well plate system. An arrangement of highly ordered 96 titania/Hydroxyapatite (TiO2/HAP) nanocomposite hollow fibers and corresponding stainless-steel needles on a Teflon plate holder were used as the extraction module. The inorganic hollow fibers were prepared via a rapid and reproducible template approach (Polypropylene hollow fiber) in combination with a sol-gel method in the presence of polyvinyl alcohol (PVA), as a network maker. The hollow fiber-shape sorbents were obtained with excellent precision by weight (RSD% = 4.98, n = 10) and length (RSD% = 1.08, n = 10) criteria. The proposed design can overcome a number of geometrically dependent drawbacks of conventional high-throughput SPME methods, mainly the ones related to sorbent amount and surface area due to possessing inner/outer surfaces without additional internal supports. The SPME platform, for the first time, was successfully applied for the extraction and preconcentration of doxorubicin from urine and water media without requiring sample preparation and free from significant matrix effect. The extracted analyte was analyzed by liquid chromatography-ion trap tandem mass spectrometry (LC-MS/MS). Highly satisfactory analytical figures of merit were obtained under optimized conditions. The limit of detection (LOD), limit of quantification (LOQ) and linearity of determination were 0.1 ng mL-1, 0.25 ng mL-1 and 0.25 to 4000 ng mL-1, respectively. The interday, intraday and inter sorbent precisions for three concentration levels ranged from 2.01 to 8.09 % (n = 3), 1.02 to 8.65 % (n = 5) and 0.99 to 1.02% (n = 15), respectively. The mean intra-well RSD value for 96 individual wells in 96-MIHF-SPME-LC-MS/MS (n = 3) at the medium concentration level was 7.81%.


Assuntos
Cromatografia Líquida/métodos , Doxorrubicina/urina , Microextração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Água/química , Adolescente , Adulto , Daunorrubicina/urina , Feminino , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Masculino , Pessoa de Meia-Idade , Concentração Osmolar , Polipropilenos/química , Porosidade , Reprodutibilidade dos Testes , Fatores de Tempo , Adulto Jovem
6.
Pain Res Manag ; 2020: 5853412, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32676136

RESUMO

This equivalence, randomized, clinical trial aimed to compare the postoperative pain of root canal therapy (RCT) with pulpotomy with mineral trioxide aggregate (PMTA) or calcium-enriched mixture (PCEM) in permanent mature teeth. In seven academic centers, 550 cariously exposed pulps were included and randomly allocated into PMTA (n = 188), PCEM (n = 194), or RCT (n = 168) arms. Preoperative "Pain Intensity" (PI) on Numerical Rating Scale and postoperative PIs until day 7 were recorded. Patients' demographic and pre-/intra-/postoperative factors/conditions were recorded/analysed. The arms were homogeneous in terms of demographics. The mean preoperative PIs were similar (P=0.998), the mean sum PIs recorded during 10 postoperative intervals were comparable (P=0.939), and the trend/changes in pain relief were parallel (P=0.821) in all study arms. The incidences of preoperative moderate-severe pain in RCT, PMTA, and PCEM arms were 56.5%, 55.7%, and 56.7%, which after 24 hours considerably decreased to 13.1%, 10.6%, and 12.9%, respectively (P=0.578). The time span of endodontic procedures was statistically different; RCT = 69.73, PMTA = 35.37, and PCEM = 33.62 minutes (P < 0.001). Patients with greater preoperative pain, symptomatic apical periodontitis, or presence of PDL widening suffered more pain (P=0.002, 0.035, and 0.023, resp.); however, other pre-/intra-/postoperative factors/conditions were comparable. Pulpotomy with MTA/CEM and RCT demonstrate comparable and effective postoperative pain relief.


Assuntos
Dor Pós-Operatória/etiologia , Pulpotomia/métodos , Materiais Restauradores do Canal Radicular/uso terapêutico , Tratamento do Canal Radicular/métodos , Adulto , Compostos de Alumínio/uso terapêutico , Compostos de Cálcio/uso terapêutico , Cimentos Dentários/uso terapêutico , Combinação de Medicamentos , Feminino , Humanos , Masculino , Dente Molar , Óxidos/uso terapêutico , Dor Pós-Operatória/epidemiologia , Prevalência , Pulpotomia/efeitos adversos , Tratamento do Canal Radicular/efeitos adversos , Silicatos/uso terapêutico , Resultado do Tratamento
7.
RSC Adv ; 10(8): 4786-4794, 2020 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-35495241

RESUMO

The structural, electronic and magnetic properties of the MIL-47(Mn) metal-organic framework are investigated using first principles calculations. We find that the large-pore structure is the ground state of this material. We show that upon transition from the large-pore to the narrow-pore structure, the magnetic ground-state configuration changes from antiferromagnetic to ferromagnetic, consistent with the computed values of the intra-chain coupling constant. Furthermore, the antiferromagnetic and ferromagnetic configuration phases have intrinsically different electronic behavior: the former is semiconducting, the latter is a metal or half-metal. The change of electronic properties during breathing posits MIL-47(Mn) as a good candidate for sensing and other applications. Our calculated electronic band structure for MIL-47(Mn) presents a combination of flat dispersionless and strongly dispersive regions in the valence and conduction bands, indicative of quasi-1D electronic behavior. The spin coupling constants are obtained by mapping the total energies onto a spin Hamiltonian. The inter-chain coupling is found to be at least one order of magnitude smaller than the intra-chain coupling for both large and narrow pores. Interestingly, the intra-chain coupling changes sign and becomes five times stronger going from the large pore to the narrow pore structure. As such MIL-47(Mn) could provide unique opportunities for tunable low-dimensional magnetism in transition metal oxide systems.

8.
Talanta ; 129: 309-14, 2014 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-25127600

RESUMO

Continuous sample drop flow-based microextraction (CSDF-ME) is an improved version of continuous-flow microextraction (CFME) and a novel technique developed for extraction and preconcentration of benzene, toluene, ethyl benzene, m-xylene and o-xylene (BTEXs) from aqueous samples prior to gas chromatography-flame ionization detection (GC-FID). In this technique, a small amount (a few microliters) of organic solvent is transferred to the bottom of a conical bottom test tube and a few mL of aqueous solution is moved through the organic solvent at relatively slow flow rate. The aqueous solution transforms into fine droplets while passing through the organic solvent. After extraction, the enriched analyte in the extraction solvent is determined by GC-FID. The type of extraction solvent, its volume, needle diameter, and aqueous sample flow rate were investigated. The enrichment factor was 221-269 under optimum conditions and the recovery was 89-102%. The linear ranges and limits of detection for BTEXs were 2-500 and 1.4-3.1 µg L(-1), respectively. The relative standard deviations for 10 µg L(-1) of BTEXs in water were 1.8-6.2% (n=5). The advantages of CSDF-ME are its low cost, relatively short sample preparation time, low solvent consumption, high recovery, and high enrichment factor.


Assuntos
Microextração em Fase Líquida/métodos , Compostos Orgânicos/química , Poluentes Químicos da Água/química , Automação , Benzeno/química , Derivados de Benzeno/química , Clorofórmio/química , Cromatografia Gasosa/métodos , Monitoramento Ambiental , Ionização de Chama/métodos , Irã (Geográfico) , Reprodutibilidade dos Testes , Rios/química , Solventes/química , Tolueno/química , Água/química , Xilenos/química
9.
Phytother Res ; 26(9): 1399-404, 2012 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-22318903

RESUMO

Linalool, a terpene alcohol, has been shown to interact with the opioid system and N-methyl-D-aspartate (NMDA) receptor. Therefore, the effect of linalool on morphine dependence and tolerance was studied. Dependence and tolerance were induced in mice using subcutaneous morphine injections, three times a day (50, 50 and 75 mg/kg /day) for 3 days. To evaluate the effect of agents on the induction of morphine dependence and tolerance, linalool (50, 75 and 100 mg/kg), clonidine (positive control), alpha-2 receptor agonist, (0.1 mg/kg), memantine, NMDA receptor antagonist (positive control), (30 mg/kg) and saline were injected intraperitoneally three times a day for 3 days. To determine the expression of morphine dependence and tolerance, all compounds were injected once intraperitoneally on the day of experiment. The effect of linalool and other agents on dependence were evaluated by counting the number of jumps (induced by naloxone 5 mg/kg). The tolerance was evaluated by the tail-flick test. The results showed that linalool in the induction and expression phase increased the nociception threshold. Linalool (48% and 95.6% at doses 75 and 100 mg/kg, respectively), clonidine and memantine reduced the severity of withdrawal signs in the induction and expression phases. This study indicated that linalool has a significant effect on morphine tolerance and dependence. This effect may be mediated partially through the inhibition of NMDA receptors.


Assuntos
Tolerância a Medicamentos , Monoterpenos/farmacologia , Dependência de Morfina/tratamento farmacológico , Monoterpenos Acíclicos , Analgésicos Opioides/farmacologia , Animais , Clonidina/farmacologia , Masculino , Camundongos , Morfina/farmacologia , Medição da Dor
10.
Anal Chim Acta ; 702(2): 274-9, 2011 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-21839209

RESUMO

In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40°C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 µL; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g(-1) and the relative standard deviations for 20 ng g(-1) of the OCPs, varied from 3.2% to 8% (n=4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.


Assuntos
Cromatografia Gasosa/métodos , Peixes/metabolismo , Hidrocarbonetos Clorados/análise , Extração Líquido-Líquido/métodos , Praguicidas/análise , Ultrassom/métodos , Acetonitrilas/química , Animais , Clorofórmio/química , Hidrocarbonetos Clorados/química , Limite de Detecção , Microquímica/métodos , Praguicidas/química , Solventes/química , Temperatura , Fatores de Tempo , Água/química
11.
Bioelectrochemistry ; 77(2): 120-4, 2010 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-19674943

RESUMO

Electrochemical oxidation of glucose on a glassy carbon disc electrode modified with multi-walled carbon nanotubes and nickel(II) oxide (GC/MWCNT/NiO) was examined by cyclic voltammetry and chronoamperometry in alkaline aqueous solutions. The results were compared with those obtained on a nickel(II) oxide modified glassy carbon electrode (GC/NiO). Both electrodes conditioned by potential cycling in a limited potential range (0.1-0.6 V vs. Ag/AgCl) in 0.10 M NaOH solution. It was found that the multi-walled carbon nanotubes improve remarkably the reactivity of nickel(II) oxide for glucose oxidation. The GC/MWCNT/NiO electrode exhibited good linear behavior in the concentration range from 2.0x10(-4) mol/L to 1.2x10(-2) mol/L for the quantitative analysis of glucose with a limit of detection of 1.6x10(-4) mol/L (3sigma). The prepared electrode exhibits satisfactory stability and long life if stored at ambient conditions. Finally, it has been demonstrated that the proposed modified electrode can be successfully used for the assay of glucose in serum samples.


Assuntos
Técnicas Eletroquímicas/instrumentação , Glucose/análise , Glucose/química , Nanotubos de Carbono/química , Níquel/química , Óxidos/química , Glicemia/análise , Técnicas Eletroquímicas/métodos , Eletrodos , Vidro/química , Concentração de Íons de Hidrogênio , Limite de Detecção , Oxirredução , Soluções/química
12.
J Hazard Mater ; 169(1-3): 907-11, 2009 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-19467774

RESUMO

In this article, a new method for the determination of organophosphorus pesticides (OPPs) in tea was developed by using dispersive liquid-liquid microextraction (DLLME) and gas chromatography-flame photometric detection (GC-FPD). A mixture of acetonitrile and n-hexane was used as an extraction solvent for the extraction of OPPs from tea samples. When the extraction process was finished, the mixture of solvents was rapidly dispersed in water; target analyte was extracted to a small volume of n-hexane, using DLLME. Recovery tests were performed for concentration 5.0 microg/kg. The recovery for each target analyte was in the range between 83.3 and 117.4%. The repeatability of the proposed method, expressed as relative standard deviation, varied between 3 and 7.8% (n=3). The detection limit of the method for tea was found ranging from 0.030 to 1 microg/kg for all the target pesticides. Compared with the conventional sample preparation method, the proposed method has the advantage of being quick and easy to operate, and has high-enrichment factors and low consumption of organic solvent.


Assuntos
Fracionamento Químico/métodos , Praguicidas/análise , Chá/química , Cromatografia Gasosa , Contaminação de Alimentos/análise , Compostos Organofosforados/análise , Compostos Organofosforados/isolamento & purificação , Praguicidas/isolamento & purificação , Solventes
13.
Arch Iran Med ; 12(3): 225-31, 2009 May.
Artigo em Inglês | MEDLINE | ID: mdl-19400598

RESUMO

BACKGROUND: Hepatitis B virus infection is a very common cause of chronic liver disease worldwide. It is estimated that 3% of Iranians are chronically infected with hepatitis B virus. Current population-based studies on both rural and urban prevalence of hepatitis B virus infection in Iran are sparse with results that do not always agree. We performed this study to find the prevalence of hepatitis B surface antigen, anti-hepatitis B core antibody, and associated factors in the general population of three provinces of Iran. METHODS: We randomly selected 6,583 subjects from three provinces in Iran, namely Tehran, Golestan, and Hormozgan. The subjects were aged between 18 and 65 years. Serum samples were tested for hepatitis B surface antigen and anti-hepatitis B core antibody. Various risk factors were recorded and multivariate analysis was performed. RESULTS: The prevalence of hepatitis B surface antigen and anti-hepatitis B core antibody in Iran was 2.6% and 16.4%, respectively. Predictors of hepatitis B surface antigen or anti-hepatitis B core antibody in multivariate analysis included older age, not having high-school diploma, living in a rural area, and liver disease in a family member. We did not find any significant differences between males and females. CONCLUSION: In spite of nationwide vaccination of newborns against hepatitis B virus since 1992, hepatitis B virus infection remains a very common cause of chronic liver disease in Iran which should be dealt with for at least the next 30-50 years.


Assuntos
Anticorpos Anti-Hepatite B/análise , Antígenos de Superfície da Hepatite B/análise , Vírus da Hepatite B/imunologia , Hepatite B/epidemiologia , Vigilância da População , Adolescente , Adulto , Distribuição por Idade , Idoso , Estudos Transversais , Feminino , Hepatite B/imunologia , Hepatite B/virologia , Humanos , Irã (Geográfico)/epidemiologia , Masculino , Pessoa de Meia-Idade , Prevalência , Distribuição por Sexo , Adulto Jovem
14.
Talanta ; 72(2): 387-93, 2007 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-19071629

RESUMO

In this study, a simple, rapid and efficient method, dispersive liquid-liquid microextraction (DLLME) combined gas chromatography-electron capture detection (GC-ECD), for the determination of chlorobenzenes (CBs) in water samples, has been described. This method involves the use of an appropriate mixture of extraction solvent (9.5 microl chlorobenzene) and disperser solvent (0.50 ml acetone) for the formation of cloudy solution in 5.00 ml aqueous sample containing analytes. After extraction, phase separation was performed by centrifugation and the enriched analytes in sedimented phase were determined by gas chromatography-electron capture detection (GC-ECD). Our simple conditions were conducted at room temperature with no stiring and no salt addition in order to minimize sample preparation steps. Parameters such as the kind and volume of extraction solvent, the kind and volume of disperser solvent, extraction time and salt effect, were studied and optimized. The method exhibited enrichment factors and recoveries ranging from 711 to 813 and 71.1 to 81.3%, respectively, within very short extraction time. The linearity of the method ranged from 0.05 to 100 microgl(-1) for dichlorobenzene isomers (DCB), 0.002-20 microgl(-1) for trichlorobenzene (TCB) and tetrachlorobenzene (TeCB) isomers and from 0.001 to 4 microgl(-1) for pentachlorobenzene (PeCB) and hexachlorobenzene (HCB). The limit of detection was in the low microgl(-1) level, ranging between 0.0005 and 0.05 microgl(-1). The relative standard deviations (R.S.D.s) for the concentration of DCB isomers, 5.00 microgl(-1), TCB and TeCB isomers, 0.500 microgl(-1), PeCB and HCB 0.100 microgl(-1) in water by using the internal standard were in the range of 0.52-2.8% (n=5) and without the internal standard were in the range of 4.6-6.0% (n=5). The relative recoveries of spiked CBs at different levels of chlorobenzene isomers in tap, well and river water samples were 109-121%, 105-113% and 87-120%, respectively. It is concluded that this method can be successfully applied for the determination of CBs in tap, river and well water samples.

15.
J Chromatogr A ; 1123(1): 1-9, 2006 Aug 04.
Artigo em Inglês | MEDLINE | ID: mdl-16716329

RESUMO

A new method was used for the extraction of organophosphorus pesticides (OPPs) from water samples: dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-flame photometric detection (GC-FPD). In this extraction method, a mixture of 12.0 microL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected into the 5.00 mL water sample by syringe. Thereby, a cloudy solution is formed. In fact, the cloudy state is because of the formation of fine droplets of chlorobenzene, which has been dispersed among the sample solution. In this step, the OPPs in water sample are extracted into the fine droplets of chlorobenzene. After centrifuging (2 min at 5000 rpm), the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (5.0+/-0.3 microL). Sedimented phase (0.50 microl) is injected into the GC for separation and determination of OPPs. Some important parameters, such as kind of extraction and disperser solvent and volume of them, extraction time, temperature and salt effect were investigated. Under the optimum conditions, the enrichment factors and extraction recoveries were high and ranged between 789-1070 and 78.9-107%, respectively. The linear range was wide (10-100,000 pg/mL, four orders of magnitude) and limit of detections were very low and were between 3 to 20 pg/mL for most of the analytes. The relative standard deviations (RSDs) for 2.00 microg/L of OPPs in water with internal standard were in the range of 1.2-5.6% (n=5) and without internal standard were in the range of 4.6-6.5%. The relative recoveries of OPPs from river, well and farm water at spiking levels of 50, 500 and 5000 pg/mL were 84-125, 88-123 and 93-118%, respectively. The performance of proposed method was compared with solid-phase microextraction (SPME) and single drop microextraction. DLLME is a very simple and rapid (less than 3 min) method, which requires low volume of sample (5 mL). It also has high enrichment factor and recoveries for extraction of OPPs from water.


Assuntos
Cromatografia Gasosa/métodos , Compostos Organofosforados/análise , Praguicidas/análise , Poluentes Químicos da Água/análise , Padrões de Referência , Sensibilidade e Especificidade
16.
J Chromatogr A ; 1116(1-2): 1-9, 2006 May 26.
Artigo em Inglês | MEDLINE | ID: mdl-16574135

RESUMO

A new microextraction technique termed dispersive liquid-liquid microextraction (DLLME) was developed. DLLME is a very simple and rapid method for extraction and preconcentration of organic compounds from water samples. In this method, the appropriate mixture of extraction solvent (8.0 microL C2Cl4) and disperser solvent (1.00 mL acetone) are injected into the aqueous sample (5.00 mL) by syringe, rapidly. Therefore, cloudy solution is formed. In fact, it is consisted of fine particles of extraction solvent which is dispersed entirely into aqueous phase. After centrifuging, the fine particles of extraction solvent are sedimented in the bottom of the conical test tube (5.0 +/- 0.2 microL). The performance of DLLME is illustrated with the determination of polycyclic aromatic hydrocarbons (PAHs) in water samples by using gas chromatography-flame ionization detection (GC-FID). Some important parameters, such as kind of extraction and disperser solvent and volume of them, and extraction time were investigated. Under the optimum conditions the enrichment factor ranged from 603 to 1113 and the recovery ranged from 60.3 to 111.3%. The linear range was 0.02-200 microg/L (four orders of magnitude) and limit of detection was 0.007-0.030 microg/L for most of analytes. The relative standard deviations (RSDs) for 2 microg/L of PAHs in water by using internal standard were in the range 1.4-10.2% (n = 5). The recoveries of PAHs from surface water at spiking level of 5.0 microg/L were 82.0-111.0%. The ability of DLLME technique in the extraction of other organic compounds such as organochlorine pesticides, organophosphorus pesticides and substituted benzene compounds (benzene, toluene, ethyl benzene, and xylenes) from water samples were studied. The advantages of DLLME method are simplicity of operation, rapidity, low cost, high recovery, and enrichment factor.


Assuntos
Compostos Policíclicos/isolamento & purificação , Poluentes Químicos da Água/isolamento & purificação , Cromatografia Gasosa , Compostos Policíclicos/análise , Padrões de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Solventes , Poluentes Químicos da Água/análise
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