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Master's Dissertation
DOI
https://doi.org/10.11606/D.43.2007.tde-23082007-091608
Document
Author
Full name
Suene Bernardes dos Santos
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2007
Supervisor
Committee
Tabacniks, Manfredo Harri (President)
Yoshimura, Elisabeth Mateus
Zamboni, Cibele Bugno
Title in Portuguese
Elementos traço em soro sanguíneo medidos pelos métodos PIXE e ICP-MS
Keywords in Portuguese
Elementos traço
ICP
PIXE
Soro
Abstract in Portuguese
O principal objetivo deste trabalho foi desenvolver uma metodologia de análise de soro sanguíneo utilizando os métodos Proton Induced X-ray Emission (PIXE) e Inductively Coupled Plasma Mass Spectrometry (ICP-MS). O PIXE é um método de análise multielementar baseado na detecção dos raios-X característicos emitidos pelas amostras, quando bombardeadas com feixes de íons (H+, He+, ...) com energia da ordem de alguns MeV. Já o ICP-MS é um espectrômetro de massa que analisa componentes de amostras ionizadas, separados de acordo com suas razões massa carga (m/z). Para a realização deste estudo, as amostras de sangue dos voluntários (30 jovens com idade entre 18 e 25 anos) foram coletadas no Hospital Universitário da USP utilizando tubos de vidro da BD VacutainerTM sem aditivos (Processo do Comitê de Ética: HU-615/05). O soro foi obtido pela centrifugação dos tubos a 3000 rpm. As amostras foram pipetadas sobre Nuclepore (10?m de espessura) e secas a temperatura ambiente, para o método PIXE, e diluídas de 1:10, para as análises com ICP-MS. A acurácia dos resultados foi verificada analisando materiais de referências de soro do National Institute of Public Health - Québec (ICP-03B-02 e ICP-02-S-05). A análise dos padrões apresentou 78% dos dados entre ±1?, 14% entre ±2? e 4% além de ±3?. Este estudo de elementos traço em soro humano revelou um total de 22 elementos: Be, Al, P, S, Cl, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Mo, Cd, Sn, Tl e Pb, com concentrações entre 9 ng/l e 6 g/l, o que compreende 9 ordens de grandeza, e também permitiu o estudo das funções de distribuição de probabilidades dos elementos. As técnicas utilizadas foram eficientes e complementares na realização deste trabalho. Os resultados das concentrações elementares medidas neste trabalho concordaram com os valores da literatura.
Title in English
Trace elements in serum measured by PIXE and ICP-MS
Keywords in English
ICP-MS
PIXE
serum
Trace elements
Abstract in English
The main objective of this work was to develop a methodology for the analysis of blood serum by Proton Induced X-ray Emission (PIXE) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). PIXE is a multi elementary spectrometric method that relies on the detection of characteristics X-rays emitted by a sample bombarded with an energetic (~MeV) ion beam (H+, He+, ...). With the ICP-MS one measures the elementary components in an ionised sample, separated according to their mass to charge ratio (m/z). For this study, the blood samples were collected from 30 young healthy adult volunteers with age between 18 and 25 years, in the University Hospital using additiveless BD VacutainerTM tubes (Authorisation agreement HU-615/05). Blood serum was obtained by centrifugation of the tubes at 3000 rpm. For PIXE analysis, the serum samples were pipetted on Nuclepore film (10?m thick) and dried at room temperature. For the ICP-MS analysis, the serum samples were diluted 1:10. Accuracy of both methods was obtained analysing serum reference materials supplied by the National Institute of Public Health - Québec (ICP-03B-02 and ICP-02-S-05). The analysis of the reference materials presented results for the elementary concentrations within ±1? for 78% of the data, 14% of the data lied within ±1? and ±2?, and 4% above ±3?. The analysis of trace elements in human blood serum by PIXE and ICP-MS revealed a total of 22 elements, ranging over 9 orders of magnitude: Be, Al, P, S, Cl, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Mo, Cd, Sn, Tl e Pb, with concentrations between 9 ng/l and 6 g/l. The PIXE and ICP-MS techniques were efficient and complimentary for the accomplishment of this work. The elementary concentrations measured in this work agreed with overall data in literature.
 
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Tese_suene_2007.pdf (1.98 Mbytes)
Publishing Date
2007-09-11
 
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