Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis
ABSTRACT A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted digestion of the samples in a pressurized system, red...
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Academia Brasileira de Ciências
2016-01-01
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author | MANUELLE C. CARDOZO DANNUZA D. CAVALCANTE DANIEL L.F. SILVA WALTER N.L. DOS SANTOS MARCOS A. BEZERRA |
author_facet | MANUELLE C. CARDOZO DANNUZA D. CAVALCANTE DANIEL L.F. SILVA WALTER N.L. DOS SANTOS MARCOS A. BEZERRA |
author_sort | MANUELLE C. CARDOZO |
collection | DOAJ |
description | ABSTRACT A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted digestion of the samples in a pressurized system, reduction of Sb5+ to Sb3+ with KI solution (10% w/v) in ascorbic acid (2%, w/v) and its subsequent determination by hydride generation atomic fluorescence spectrometry (HG-AFS). The proportions of each component (HCl, HNO3 and water) used in the digestion were studied applying a constrained mixtures design. The optimal proportions found were 50% water, 25% HNO3 and 25% HCl. Variables involved in the generation of antimony hydride were optimized using a Doehlert design revealing that good sensitivity is found when using 2.0% w/v NaBH4 and 4.4 mol L-1 HCl. Under the optimum experimental conditions, the method allows the determination of antimony in hair samples with detection and quantification limits of 1.4 and 4.6 ng g-1, respectively, and precision expressed as relative standard deviation (RSD) of 2.8% (n = 10 to 10.0 mg L-1). The developed method was applied in the analysis of hair samples from patients who take medication against Leishmaniasis. |
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publishDate | 2016-01-01 |
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series | Anais da Academia Brasileira de Ciências |
spelling | doaj.art-d3112195f7c9483c930ee85f77d4fa812022-12-22T01:25:26ZengAcademia Brasileira de CiênciasAnais da Academia Brasileira de Ciências1678-26902016-01-01010.1590/0001-3765201620150250S0001-37652016005013105Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against LeishmaniasisMANUELLE C. CARDOZODANNUZA D. CAVALCANTEDANIEL L.F. SILVAWALTER N.L. DOS SANTOSMARCOS A. BEZERRAABSTRACT A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted digestion of the samples in a pressurized system, reduction of Sb5+ to Sb3+ with KI solution (10% w/v) in ascorbic acid (2%, w/v) and its subsequent determination by hydride generation atomic fluorescence spectrometry (HG-AFS). The proportions of each component (HCl, HNO3 and water) used in the digestion were studied applying a constrained mixtures design. The optimal proportions found were 50% water, 25% HNO3 and 25% HCl. Variables involved in the generation of antimony hydride were optimized using a Doehlert design revealing that good sensitivity is found when using 2.0% w/v NaBH4 and 4.4 mol L-1 HCl. Under the optimum experimental conditions, the method allows the determination of antimony in hair samples with detection and quantification limits of 1.4 and 4.6 ng g-1, respectively, and precision expressed as relative standard deviation (RSD) of 2.8% (n = 10 to 10.0 mg L-1). The developed method was applied in the analysis of hair samples from patients who take medication against Leishmaniasis.http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0001-37652016005013105&lng=en&tlng=enLeishmaniasisantimonyhairHG-AFSmultivariate optimization |
spellingShingle | MANUELLE C. CARDOZO DANNUZA D. CAVALCANTE DANIEL L.F. SILVA WALTER N.L. DOS SANTOS MARCOS A. BEZERRA Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis Anais da Academia Brasileira de Ciências Leishmaniasis antimony hair HG-AFS multivariate optimization |
title | Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis |
title_full | Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis |
title_fullStr | Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis |
title_full_unstemmed | Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis |
title_short | Multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against Leishmaniasis |
title_sort | multivariate optimization of a method for antimony determination by hydride generation atomic fluorescence spectrometry in hair samples of patients undergoing chemotherapy against leishmaniasis |
topic | Leishmaniasis antimony hair HG-AFS multivariate optimization |
url | http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0001-37652016005013105&lng=en&tlng=en |
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