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1.
J Prev Alzheimers Dis ; 11(2): 453-462, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38374752

RESUMO

BACKGROUND: Cardiovascular risk factors are associated with Alzheimer's Disease (AD) development. However, few studies compare the overall cardiovascular risk with AD biomarkers, and when done, they are mainly performed in moderate cardiovascular risk regions. OBJECTIVES: To determine whether cardiovascular risk in older adults is associated with pathological cerebrospinal fluid (CSF) biomarkers of AD in a low cardiovascular risk population. DESIGN: This is a cross-sectional study performed between 2017 and 2020. PARTICIPANTS: The present work included patients between 50 and 75 years old who were negative for CSF AD biomarkers and had minimum cognitive alterations (controls) and patients with positive CSF AD biomarkers and in early stages of AD (cases). MEASUREMENTS: CSF biomarkers included total tau, phosphorylated tau 181 and amyloid ß42 (Aß42). Analytical variables were obtained. ERICE, SCORE2 and Framingham scales were used to calculate the overall patient's cardiovascular risk. The Aß42/Aß40 ratio and neurofilaments were explored when available. RESULTS: Two hundred and thirty-three patients were included. Nearly 76% of the sample had AD. AD patients had higher cardiovascular risk than controls (p-value < 0.05). ERICE and SCORE2 were associated with AD presence. Framingham was not. A correlation between elevated cardiovascular risk and higher total tau and NfL levels was observed when adjusted by age. CONCLUSION: Cardiovascular risk assessment may be helpful in neurodegenerative disorders detection, as it is associated with CSF total tau and NfL. ERICE and SCORE2 may be useful scales in low cardiovascular risk regions to improve cardiovascular control and prevent neurodegenerative pathologies.


Assuntos
Doença de Alzheimer , Doenças Cardiovasculares , Humanos , Idoso , Pessoa de Meia-Idade , Doença de Alzheimer/psicologia , Peptídeos beta-Amiloides/líquido cefalorraquidiano , Estudos Transversais , Fatores de Risco , Biomarcadores/líquido cefalorraquidiano , Fatores de Risco de Doenças Cardíacas
2.
Neurologia (Engl Ed) ; 38(4): 262-269, 2023 May.
Artigo em Inglês | MEDLINE | ID: mdl-37031800

RESUMO

We performed a retrospective analysis of the patients assessed at our memory unit for whom Alzheimer disease (AD) cerebrospinal fluid biomarker results were available. We selected patients diagnosed with mild cognitive impairment due to AD (National Institute on Aging-Alzheimer's Association clinical criteria), confirmed neuropsychological deficit, a Global Deterioration Scale score of 3, and an abnormal profile of cerebrospinal fluid biomarkers. Of the 588 cases reviewed, 110 met the inclusion criteria. During follow-up, 50 cases (45.45%) progressed to dementia due to AD. Baseline levels of total and phosphorylated tau were higher in the group of patients that progressed to dementia than in those remaining with mild cognitive impairment. After adjusting for age, sex, history of hypertension, diabetes, and educational level, a 10% increase in total tau protein values was associated with a 7.60% increase in the risk of progression to dementia (hazard ratio: 2.22; 95% confidence interval, 1.28-3.84]; P = .004). Among patients with mild cognitive impairment due to AD and abnormal cerebrospinal fluid biomarker profiles, progressively higher concentrations of total or phosphorylated tau were associated with increased risk of progression to dementia.


Assuntos
Doença de Alzheimer , Disfunção Cognitiva , Humanos , Doença de Alzheimer/diagnóstico , Prognóstico , Estudos Retrospectivos , Peptídeos beta-Amiloides , Progressão da Doença , Disfunção Cognitiva/etiologia , Disfunção Cognitiva/diagnóstico , Biomarcadores/líquido cefalorraquidiano
3.
Biol Psychol ; 177: 108511, 2023 02.
Artigo em Inglês | MEDLINE | ID: mdl-36716987

RESUMO

BACKGROUND: Emotion recognition is often impaired in early Alzheimer's disease (AD) and can be evaluated using the Reading the Mind in the Eyes Test (RMET). Similarly, cortisol levels can affect cognition and could be considered a biomarker of AD. OBJECTIVES: The aim of this study was to analyse the relationship between the emotion recognition task and cortisol levels in participants with early Alzheimer Disease (AD). METHODS: Complex emotion recognition was assessed with RMET, and plasma cortisol levels were determined by mass spectrometry in participants classified into mild cognitive impairment (MCI) due to AD (n = 25), mild dementia (MD) due to AD (n = 20), MCI non-AD (n = 34), MD non-AD (n = 13) and healthy controls (HC) (n = 16) groups. RESULTS: Significantly lower positive emotion recognition was found in the MCI non-AD group (p = 0.02) and lower emotion recognition in MD (AD and non-AD) groups (p < 0.01) compared to the healthy group. In addition, significant differences were observed between cortisol and all RMET scores among the MCI and MD groups (p < 0.01). A significant correlation was also obtained between total and neutral RMET scores and cortisol levels in MD groups (p = 0.01). CONCLUSIONS: These outcomes suggest that detection of positive emotion dysfunction could help to identify MCI non-AD patients. Furthermore, general impaired emotion recognition and high cortisol levels may be associated with cognitive impairment at mild dementia level.


Assuntos
Doença de Alzheimer , Disfunção Cognitiva , Demência , Humanos , Doença de Alzheimer/diagnóstico , Doença de Alzheimer/psicologia , Hidrocortisona , Emoções
4.
Public Health ; 210: 142-148, 2022 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-35970016

RESUMO

OBJECTIVES: The acquisition of emotional competencies through emotional education programs improves both short- and long-term health outcomes. The 1,2,3,emoció! program directed at children aged 3-5 years aims to promote health through the development of emotional competencies. This study evaluated the effectiveness of the program during its first year of implementation. STUDY DESIGN: Cluster randomized trial. METHODS: The information sources were an ad-hoc questionnaire to evaluate emotional competencies and focus group discussions with the teachers implementing the program. For the quantitative data analysis, we compared mean emotional competencies scores pre- and postintervention for the intervention group and the comparison group. We also conducted a multilevel regression with repeated measures, adjusted by sociodemographic variables and stratified by gender and school year. For the qualitative data, we performed a thematic content analysis. RESULTS: The sample consisted of 2625 children (48.4% girls and 49.2% intervention group). Emotional competencies improved in both groups after the school year (P-value < 0.001), but the increase was greater in the intervention group. The multilevel analysis showed an improvement in the final scores attributed to the intervention, especially for those in the first year of preschool [boys: 12.33 points (95% CI 5.51-19.15), girls: 9.66 points (95% CI 3.36-15.96)]. The thematic content analysis also highlighted enhanced emotional competencies in the intervention group. The final scores did not vary by sociodemographic variables. CONCLUSIONS: The 1,2,3,emoció! program had a positive effect on emotional competencies among children, with effectivity being higher among younger children.


Assuntos
Promoção da Saúde , Instituições Acadêmicas , Criança , Pré-Escolar , Cognição , Emoções , Feminino , Humanos , Masculino , Avaliação de Programas e Projetos de Saúde , Inquéritos e Questionários
5.
Farm. comunitarios (Internet) ; 14(Supl 1): 1, junio 2022. ilus, tab
Artigo em Espanhol | IBECS | ID: ibc-209348

RESUMO

JUSTIFICACIÓN: la farmacia comunitaria atiende regularmente a pacientes de edad avanzada, lo que le permite detectar cambios anómalos en la conducta. Ofrecer resultados de escalas cognitivas a atención primaria, con tiempo limitado por paciente, podría facilitar la detección de casos de deterioro cognitivo (DC) y disminuir el tiempo de diagnóstico.OBJETIVOS: elaborar un protocolo que facilite la colaboración médico-farmacéutico efectiva, capaz de detectar de manera precoz el DC y de disminuir el tiempo de diagnóstico.MATERIAL Y MÉTODOS: se establecen dos grupos: un grupo de colaboración interprofesional (IPC), n=26 farmacias y otro sin colaboración interprofesional (No-IPC), n=9 farmacias. Se facilita a las farmacias IPC material y formación para detectar pacientes con posible DC mediante la plataforma de un Colegio Oficial de Farmacéuticos. Simultáneamente, se contacta con los centros de salud y hospitales pertenecientes a dichas áreas y se les explica el protocolo, valorando la derivación de pacientes de fuera de su área de salud en caso necesario. Se designa a un coordinador que facilita la comunicación entre los centros y seguimiento de los pacientes, elaborándose una campaña de comunicación del proyecto. En el grupo No-IPC, no se facilitan los recursos ni la coordinación mencionada previamente. Las diferencias entre los grupos respecto a la detección eficaz de pacientes con alta probabilidad de presentar DC han sido analizadas estadísticamente mediante el test chi-cuadrado mediante el programa R Commander. Este trabajo ha sido aprobado por dos Comités Éticos, bajo los registros, CEI18/027 y MOR-ROY-2018- 013. Todos los pacientes firmaron el consentimiento informado.RESULTADOS/DISCUSIÓN: se han cribado 349 pacientes en las farmacias IPC y 138 pacientes en las farmacias No-IPC. (AU)


Assuntos
Humanos , Demência , Atenção Primária à Saúde , Disfunção Cognitiva , Farmácia , Pacientes
6.
Neurologia (Engl Ed) ; 2020 Oct 31.
Artigo em Inglês, Espanhol | MEDLINE | ID: mdl-33143865

RESUMO

We performed a retrospective analysis of the patients assessed at our memory unit for whom Alzheimer disease (AD) cerebrospinal fluid biomarker results were available. We selected patients diagnosed with mild cognitive impairment due to AD (National Institute on Aging-Alzheimer's Association clinical criteria), confirmed neuropsychological deficit, a Global Deterioration Scale score of 3, and an abnormal profile of cerebrospinal fluid biomarkers. Of the 588 cases reviewed, 110 met the inclusion criteria. During follow-up, 50 cases (45.45%) progressed to dementia due to AD. Baseline levels of total and phosphorylated tau were higher in the group of patients that progressed to dementia than in those remaining with mild cognitive impairment. After adjusting for age, sex, history of hypertension, diabetes, and educational level, a 10% increase in total tau protein values was associated with a 7.60% increase in the risk of progression to dementia (hazard ratio: 2.22; 95% confidence interval, 1.28-3.84]; P = .004). Among patients with mild cognitive impairment due to AD and abnormal cerebrospinal fluid biomarker profiles, progressively higher concentrations of total or phosphorylated tau were associated with increased risk of progression to dementia.

7.
Exp Gerontol ; 123: 10-16, 2019 08.
Artigo em Inglês | MEDLINE | ID: mdl-31117002

RESUMO

Cortisol dysregulation is proposed as a factor in the development of Alzheimer's disease (AD). AD patients can show high cortisol levels in prodromal phases of AD, early enough that neuropsychological alterations exist but activities of daily living remain unimpaired. Nevertheless, it is unknown if biofluid cortisol levels can have some AD predictive power together with neuropsychological assessment in prodromal stages in comparison with other cognitive disorders. In this work, an analytical method based on ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was applied to determine the cortisol levels in different biofluids (urine, plasma, saliva, cerebrospinal fluid). Early AD patients and non-AD patients recruited at out-patient neurological unit were classified from the standard cerebrospinal fluid biomarkers levels (ß-amyloid, tau, phosphorylated tau), and studied with an extensive neuropsychological assessment including global, neuropsychological, functional and affective scales. We used a logistic regression model to discriminate between the AD and non-AD groups. Higher plasma cortisol levels were found in the AD group than in the non-AD group (p < 0.001). Regarding neuropsychological evaluation, delayed memory was used as representative of the neuropsychological status, and lower scores were obtained in the AD group (p < 0.001). The prediction model, including plasma cortisol levels and delayed memory scores, achieved an AUC of 0.93, as well as a sensitivity of 97% and a specificity of 69.4%. In conclusion, plasma cortisol levels and delayed memory scores were specifically impaired in early AD, allowing the development of a new diagnostic model which could be employed as a very satisfactory screening system.


Assuntos
Atividades Cotidianas , Doença de Alzheimer , Hidrocortisona/sangue , Testes Neuropsicológicos , Repressão Psicológica , Idoso , Doença de Alzheimer/diagnóstico , Doença de Alzheimer/metabolismo , Doença de Alzheimer/psicologia , Peptídeos beta-Amiloides/líquido cefalorraquidiano , Biomarcadores/sangue , Biomarcadores/líquido cefalorraquidiano , Biomarcadores/urina , Feminino , Humanos , Hidrocortisona/líquido cefalorraquidiano , Hidrocortisona/urina , Masculino , Pessoa de Meia-Idade , Valor Preditivo dos Testes , Espectrometria de Massas em Tandem/métodos , Proteínas tau/líquido cefalorraquidiano
8.
Semin Fetal Neonatal Med ; 24(4): 101002, 2019 08.
Artigo em Inglês | MEDLINE | ID: mdl-30981693

RESUMO

The neonatal period is a highly sensitive time span during which stressful experiences may have an influence on later health outcomes. Medical procedures applied to newborn babies during hospitalization are stressors that trigger a physiological and psychological stress response. Stress response has been traditionally evaluated using scores based on behavioural signs such as facial expressions, limb movements, crying, etc., which are subjectively interpreted. Only few studies have employed measurable physiological signs to objectively evaluate the stress response to specific interventions. The aim of this review is to inform of recently developed biochemical methods that allow clinicians to evaluate the stress response to medical procedures performed in the neonatal period in biological samples non-invasively obtained. Stress biomarkers are based on the physiological stress response mediated by the hypophysis-pituitary-adrenal axis and the sympathetic-adreno-medullary systems. Cortisol is at present the most widely employed laboratory determination to measure stress levels. In recent years, sequentially determined salivary cortisol levels have allowed non-invasive monitoring of newborn infants under stressful conditions in the NICU.


Assuntos
Biomarcadores/metabolismo , Estresse Fisiológico , Estresse Psicológico/diagnóstico , 17-alfa-Hidroxiprogesterona/metabolismo , Catecolaminas/metabolismo , Citocinas/metabolismo , Glicopeptídeos/metabolismo , Cabelo/metabolismo , Humanos , Hidrocortisona/metabolismo , Recém-Nascido , Unidades de Terapia Intensiva Neonatal , Peróxidos Lipídicos/metabolismo , Norepinefrina/metabolismo , Ocitocina/metabolismo , Saliva/metabolismo , alfa-Amilases/metabolismo
9.
Talanta ; 153: 152-7, 2016 06 01.
Artigo em Inglês | MEDLINE | ID: mdl-27130102

RESUMO

This paper describes a reliable analytical method based on ultra-performance liquid chromatography coupled to tandem mass spectrometry to determine F2-isoprostanes and other total byproducts (isoprostanes, isofurans, neuroprostanes and neurofurans) as lipid peroxidation biomarkers in newborn plasma samples. The proposed procedure is characterized by a simple sample treatment employing a reduced sample volume (100µL). Also, it shows a high throughput and high selectivity to determine simultaneously different isoprostane isomers in a large number of samples. The reliability of the described method was demonstrated by analysis of spiked plasma samples, obtaining recoveries between 70% and 130% for most of the analytes. Taking into account the implementation of further clinical studies, it was demonstrated the proper sensitivity of the method by means of the analysis of few human newborn plasma samples. In addition to this, newborn piglet plasma samples (n=80) were analyzed observing that the developed method was suitable to determine the analyte levels present in this kind of samples. Therefore, this analytical method could be applied in further clinical research about establishment of reliable lipid peroxidation biomarkers employing this experimental model.


Assuntos
Peroxidação de Lipídeos , Biomarcadores , Humanos , Recém-Nascido , Isoprostanos , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem
10.
Anal Chim Acta ; 886: 214-20, 2015 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-26320656

RESUMO

Byproducts of arachidonic (AA) and docosahexaenoic acid (DHA) oxidation are highly relevant for the study of free radical associated conditions in the perinatal period. Plasma metabolites can provide the clinician with a snapshot of the oxidant status of patients before and after specific clinical interventions (e.g.: supplementation with oxygen). We describe a new andreliable ultra-performance liquid mass spectrometry method to determine F2-isoprostanes and other byproducts (isoprostanes, isofurans, neuroprostanes, neurofurans) in newborn serum samples. Cord blood samples were obtained from severely depressed newborn infants (Apgar score 1 min < 3; arterial cord pH < 7.00), and aliquoted for serum determination and stored at -80 °C. A UHPLC-MS/MS method was employed. It has a series of technical advantages: simple sample treatment; reduced sample volume (100 µL) which is essential for preterm neonates with low circulating blood volume, high throughput of sample analysis (96 samples in less than 24 h) and high selectivity for different isoprostanes isomers. Excellent sensitivity was achieved within limits of detection between 0.06 and 4.2 nmol L(-1), which renders this method suitable to monitoranalyte concentration in newborn samples. The method's precision was satisfactory; with coefficients of variation around 5-12% (intra-day) and 7-17% (inter-day). The reliability of the described method was assessed by analysis of spiked serum samples obtaining recoveries between 70% and 120%. The proposed method has rendered suitable for serum determination for newborn babies at risk of oxygen free radical associated conditions.


Assuntos
Biomarcadores/sangue , Cromatografia Líquida de Alta Pressão/métodos , Peroxidação de Lipídeos , Lipídeos/sangue , Estresse Oxidativo , Espectrometria de Massas em Tandem/métodos , Humanos , Recém-Nascido/sangue , Limite de Detecção
11.
Anal Bioanal Chem ; 394(2): 557-65, 2009 May.
Artigo em Inglês | MEDLINE | ID: mdl-19255747

RESUMO

This paper describes a cost-effective procedure for the analysis of short-chain aliphatic amines in water samples using a solid-phase microextraction device. Analyte preconcentration and derivatisation were effected into a capillary column coated with 95% polydimethylsiloxane-5% polydiphenylsiloxane, which was used as the injection loop of a Rheodyne injection valve. The coating was previously loaded with the derivatisation reagent, 9-fluorenylmethyl chloroformate. A volume of 1 mL of samples was then drawn into the capillary column, and the extracted analytes were left to react on the capillary coating for 5 min. Next, the capillary column was cleaned by passing water. Finally, the injection valve was rotated, and the derivatives formed were dynamically desorbed and transferred to the analytical column into the mobile phase. Methylamine, ethylamine, propylamine, n-butylamine and n-pentylamine were selected as model compounds. Excellent sensitivity was achieved, being the limits of detection of 15-200 microg/L when using UV detection and of 0.1-0.4 microg/L by fluorescence.

12.
J Chromatogr A ; 1188(2): 118-23, 2008 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-18329653

RESUMO

A method for the analysis of dimethylamine (DMA) by automated in-tube solid-phase microextraction (IT-SPME)-supported chemical derivatization coupled with high-performance liquid chromatography was developed. Extraction, derivatization and desorption were studied by using a capillary coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane. Solution derivatization and automated IT-SPME derivatization using 9-fluorenylmethyl chloroformate (FMOC) were compared. The proposed procedure provided adequate linearity, accuracy and precision in the 0.2-2.0 microg/mL concentration interval, and the limit of detection (LOD) was 50 ng/mL. The main advantages of the proposed procedure are: (i) no off-line sample manipulation, (ii) rapidity, as the total analysis time is about 10 min, (iii) specificity for the samples assayed, (iv) minimal consumption of FMOC reagent and (v) minimal residues. Therefore, the proposed method is an environmental-friendly and cost-effective alternative for the control of residual DMA in polymeric cationic surfactants used like flocculants in water treatment.


Assuntos
Dimetilaminas/análise , Sistemas On-Line , Polímeros/química , Microextração em Fase Sólida/métodos , Cromatografia Líquida
13.
Anal Chim Acta ; 610(2): 268-73, 2008 Mar 10.
Artigo em Inglês | MEDLINE | ID: mdl-18291139

RESUMO

A 80-cm length commercially available capillary coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane (TBR-5) was employed to carry out on-line extraction and preconcentration of dibuthyl phthalate (DBP) and di-2-ethylhexyl phthalate (DEHP) in the chromatographic system. The coated capillary was placed between the sample injection loop and the injection needle of an autosampler. Variables affecting the automatic in-tube solid-phase microextraction (SPME) were optimized. A Genesis C(18) (5 cm x 4.6 mm i.d., 4 microm particle size) was employed as analytical column. The achieved limits of detection by use of diode array detection were 1 and 2.5 microg L(-1), respectively. The proposed conditions have been applied to determine those compounds at low ppb levels (< or =250 microg L(-1)) in aqueous samples. No matrix effect was found, and recoveries between 85 and 115% were obtained. The precision of the method was good, and the achieved intra- and inter-day variation coefficients were between 5 and 20%. The analysis time per sample was 20 min and any off-line pre-treatment of the samples was needed. The taken sample volume was 100 microL. Data on the application of the described method to the analysis of different water samples are presented.


Assuntos
Análise Custo-Benefício , Dibutilftalato/análise , Dietilexilftalato/análise , Poluentes Químicos da Água/análise , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
14.
J Chromatogr A ; 1141(1): 10-21, 2007 Feb 02.
Artigo em Inglês | MEDLINE | ID: mdl-17188696

RESUMO

This paper describes a method for the selective screening of organophosphorus pesticides in water. In-tube solid-phase microextraction (SPME) in an open capillary column coupled to capillary liquid chromatography (LC) with UV detection has been used to effect preconcentration, separation and detection of the analytes in the same assembly. For in-tube SPME two capillary columns of the same length and different internal diameters and coating thicknesses have been tested and compared, a 30 cm x 0.25 mm I.D., 0.25 micro m thickness coating column, and a 30 cm x 0.1 mm I.D., 0.1 micro m of coating thickness column. In both columns the coating was 95% dimethylpolysiloxane (PDMS)-5% diphenylpolysiloxane. The proposed methodology provided limits of detections (LODs) for the tested organophosphorus pesticides in the 0.1-10 micro g/L range, whereas the direct injection of the samples onto the capillary LC system provided LODs in the 50-1000 micro g/L range. The sensitivity of the proposed in-tube SPME-capillary LC method is adequate to monitorize the analyte levels in drinking water. Several triazines, polycyclic aromatic hydrocarbons (PAHs), nonylphenol, organochloride pesticides or polybrominated diphenyl ethers (PBDEs) have been evaluated as possible interferents. The reliability of the described method is demonstrated by analysing different real water samples.


Assuntos
Cromatografia Líquida/métodos , Meio Ambiente , Compostos Organofosforados/análise , Praguicidas/análise , Microextração em Fase Sólida/métodos , Água/química , Compostos Organofosforados/química , Compostos Organofosforados/isolamento & purificação , Praguicidas/química , Praguicidas/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação
15.
J Chromatogr A ; 1125(2): 159-71, 2006 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-16797563

RESUMO

This paper compares the advantages and disadvantages of two different configurations for the extraction of triazines from water samples: (1) on-fibre solid-phase microextraction (SPME) coupled to conventional liquid chromatography (LC); and (2) in-tube SPME coupled to capillary LC. In-tube SPME has been effected either with a packed column or with an open capillary column. A critical evaluation of the main parameters affecting the performance of each method has been carried out in order to select the most suitable approach according to the requirements of the analysis. In the on-fibre SPME configuration the fibre coating was polydimethylsiloxane (PDMS)-divinylbenzene (DVB). The limits of detection (LODs) obtained with this approach under the optimized extraction and desorption conditions were between 25 and 125 microg/L. The in-tube SPME approach with a C18 packed column (35 mm x 0.5 mm I.D., 5 microm particle size) connected to a switching micro-valve provided the best sensitivity; under such configuration the LODs were between 0.025 and 0.5 microg/L. The in-tube SPME approach with an open capillary column coated with PDMS (30 cm x 0.25 mm I.D., 0.25 microm of thickness coating) connected to the injection valve provided LODs between 0.1 and 0.5 microg/L. In all configurations UV detection at 230 nm was used. Atrazine, simazine, propazine, ametryn, prometryn and terbutryn were selected as model compounds.


Assuntos
Cromatografia Líquida/métodos , Triazinas/análise , Triazinas/isolamento & purificação , Água/química , Substâncias Húmicas , Triazinas/química
16.
J Chromatogr A ; 1104(1-2): 40-6, 2006 Feb 03.
Artigo em Inglês | MEDLINE | ID: mdl-16375912

RESUMO

The reliability of SPME combined with a chemical reaction for the analysis of short-chain aliphatic amines by liquid chromatography has been investigated. Different options to couple SPME and derivatization have been tested and compared: (i) derivatization of the analytes in solution followed by the extraction of the derivatives, (ii) extraction of the analytes and subsequent derivatization by immersing the SPME fibre onto a solution of the reagent, and (iii) extraction/derivatization of the analytes using fibres previously coated with the reagent. Methylamine (MA), dimethylamine (DMA) and trimethylamine (TMA) have been selected as a model of primary, secondary and tertiary amines, respectively. The analytes have been derivatized with the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC), and the fibre coating was Carbowax-templated resin (CW-TR). The employment of fibres coated with FMOC to extract and derivatize the analytes was the best option, as compared with the other approaches tested the sensitivity was considerably improved. On the basis of these studies, a new procedure for the determination of MA, DMA and TMA in water is presented. To demonstrate the utility of the proposed conditions data on linearity, accuracy, repeatability and sensitivity are given. Results of the determination of the amines in tap, river and waste water are also presented.


Assuntos
Aminas/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Fluorenos/química , Indicadores e Reagentes , Soluções
17.
J Pharm Biomed Anal ; 40(5): 1209-17, 2006 Mar 18.
Artigo em Inglês | MEDLINE | ID: mdl-16290021

RESUMO

The utility of combining chiral derivatization and solid-phase microextraction (SPME) for the enantiomeric analysis of primary amphetamines by liquid chromatography has been investigated. Different derivatization/extraction strategies have been evaluated and compared using the chiral reagent o-phthaldialdehyde (OPA)-N-acetyl-l-cysteine (NAC) and fibres with a Carbowax-templated resin coating. Amphetamine, norephedrine and 3,4-methylenedioxyamphetamine (MDA) were used as model compounds. On the basis of the results obtained, a new method is presented based on the derivatization of the analytes in solution followed by SPME of the OPA-NAC derivatives formed. The proposed conditions have been applied to determine the compounds of interest at low ppm levels (

Assuntos
Anfetaminas/análise , Estimulantes do Sistema Nervoso Central/análise , Anfetaminas/urina , Estimulantes do Sistema Nervoso Central/urina , Cromatografia Líquida de Alta Pressão , Humanos , Indicadores e Reagentes , Fenilpropanolamina/análise , Fenilpropanolamina/urina , Reprodutibilidade dos Testes , Soluções , Espectrometria de Fluorescência , Estereoisomerismo
18.
Talanta ; 69(3): 716-23, 2006 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-18970628

RESUMO

This work describes a new approach for the determination of trimethylamine (TMA) in water and air by liquid chromatography (LC). The assay is based on the employment of a solid-phase microextraction (SPME) fiber for sampling and for derivatization of the analyte with the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC). The fiber, with a Carbowax-templated resin -50mum coating, was first immersed into a solution of the reagent. Once loaded with the reagent, the fiber was immersed into the water samples or exposed to the air samples in order to extract and to derivatize the analyte. Finally, the fiber was placed into a HPLC-SPME interface to desorb and transfer the TMA-FMOC derivative to the LC equipment. A comparative study of the analytical characteristics of the procedure in water and air samples was carried out. Under optimized conditions, the proposed approach permits the quantification of TMA in solution within the 1.0-10.0mug/ml interval and in air within the 25-200mg/m(3) interval. The limits of detection were 0.25mug/ml and 12mg/m(3) (25 degrees C, 1.013x10(-5)Pa) in water and air, respectively. The utility of the proposed method for determining TMA in different kind of samples is discussed.

19.
Talanta ; 66(5): 1139-45, 2005 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-18970101

RESUMO

A new method is presented for the determination of DMA in water as its 9-fluorenylmethyl chloroformate (FMOC) derivative using solid-phase microextraction (SPME) and liquid chromatography. The method is based on the employment of SPME fibres coated with carbowax-templated resin (CW-TR) for analyte extraction and derivatization. The fibres were successively immersed in the samples, in a solution of o-phthalaldialdehyde and N-acethyl-l-cysteine (OPA-NAC) and finally, in a solution of FMOC. OPA-NAC reacted on the fibre with possible primary aliphatic amines present in the samples, particularly with PA which is a direct interferent in the determination of DMA with FMOC. In such a way, the formation of PA-FMOC during the second stage was prevented, and thus the method was selective for DMA. The proposed procedure was applied to the determination of DMA in the 1.0-10.0mug/mL range. The method provided suitable linearity, accuracy and reproducibility, and limits of detection and quantification of 0.3 and 1.0mug/mL, respectively. The applicability of the method for the determination of DMA in different types of water is shown.

20.
Anal Biochem ; 333(2): 328-35, 2004 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-15450809

RESUMO

This work evaluates the utility of solid-phase microextraction (SPME) in the analysis of amphetamines by liquid chromatography (LC) after chemical derivatization of the analytes. Two approaches have been tested and compared, SPME followed by on-fiber derivatization of the extracted amphetamines, and solution derivatization followed by SPME of the derivatives formed. Both methods have been applied to measure amphetamine (AP), methamphetamine (MA), and 3,4-methylenedioxymethamphetamine (MDMA), using the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) and carbowax-templated resin (CW-TR)-coated fibers. Data on the application of the proposed methods for the analysis of different kind of samples are presented. When analyzing aqueous solutions of the analytes, both approaches gave similar analytical performance, but the sensitivity attainable with the solution derivatization/SPME method was better. The efficiencies observed when processing spiked urine samples by the SPME/on-fiber derivatization approach were very low. This was because the extraction of matrix components into the fiber coating prevented the extraction of the reagent. In contrast, the efficiencies obtained for spiked urine samples by the solution derivatization/SPME approach were similar to those obtained for aqueous samples. Therefore, the later method would be the method of choice for the quantification of amphetamines in urine.


Assuntos
Anfetaminas/análise , Anfetaminas/química , Microquímica/métodos , Anfetaminas/isolamento & purificação , Anfetaminas/urina , Cromatografia Líquida de Alta Pressão , Valores de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
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