Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy

Lead and chromium contamination represents one of the most serious problems in the aquatic environments. The aim of this work was to develop and validate an accurate, sensitivity, and rapid method for the simultaneous determination of Pb and Cr at trace levels in tissues and fat of marine organisms...

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Main Authors: Blanca G. Beltrán, Ibiza Martínez-Serrano, Victor Ramos-Sanchez, David Chávez-Flores, Myrna C. Nevárez-Rodríguez, Emilio A. Suárez-Domínguez
Format: Article
Language:English
Published: Wiley 2019-01-01
Series:Journal of Analytical Methods in Chemistry
Online Access:http://dx.doi.org/10.1155/2019/8150678
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author Blanca G. Beltrán
Ibiza Martínez-Serrano
Victor Ramos-Sanchez
David Chávez-Flores
Myrna C. Nevárez-Rodríguez
Emilio A. Suárez-Domínguez
author_facet Blanca G. Beltrán
Ibiza Martínez-Serrano
Victor Ramos-Sanchez
David Chávez-Flores
Myrna C. Nevárez-Rodríguez
Emilio A. Suárez-Domínguez
author_sort Blanca G. Beltrán
collection DOAJ
description Lead and chromium contamination represents one of the most serious problems in the aquatic environments. The aim of this work was to develop and validate an accurate, sensitivity, and rapid method for the simultaneous determination of Pb and Cr at trace levels in tissues and fat of marine organisms such as turtle (Chelonia mydas), shark (Rhizoprionodon terraenovae), and dolphin (Tursiops truncatus), utilizing the total reflection X-Ray fluorescence (TXRF) spectroscopy. Working solutions were prepared in 10 mL of a solution 0.005 mol·L−1 EDTA and 1 mol·L−1 HNO3. In order to correct possible instrument drifts, 20 μg·L−1 of gallium was used as internal standard (IS). The results showed that TXRF method was linear over the concentration ranges of 5.242–100 μg·L−1 for Pb and 2.363–100 μg·L−1 for Cr. Limits of detection (LOD) achieved were 1.573 and 0.709 μg·L−1 for Pb and Cr, respectively, while limits of quantification achieved were 5.242 μg·L−1 for Pb and 2.363 μg·L−1 for Cr. The validated method was accurate and precise enough for determination of these heavy metals in samples of marine organisms as indicated by acceptable values of recovery between 90–101%. In addition, a certified reference material (BCR-279, sea lettuce) and a Centrum tablet were satisfactory analyzed, and the T-test for comparison of means revealed that there were no significant differences at the 95% confidence level between the values obtained with the proposed TXRF method and the certificated values. The repeatability of the method, expressed as relative standard deviation (RSD), was 5.1% and 4%, for Pb and Cr, respectively. In addition, other features of the developed method were a low sample volume of 10 μL, and the sample frequency achieved was 20 h−1.
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series Journal of Analytical Methods in Chemistry
spelling doaj-art-0e3f20aac9e74f3fbbf48817a6121e242025-02-03T01:21:42ZengWileyJournal of Analytical Methods in Chemistry2090-88652090-88732019-01-01201910.1155/2019/81506788150678Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) SpectroscopyBlanca G. Beltrán0Ibiza Martínez-Serrano1Victor Ramos-Sanchez2David Chávez-Flores3Myrna C. Nevárez-Rodríguez4Emilio A. Suárez-Domínguez5Faculty of Nursing and Nutriology, Chihuahua Autonomous University, C.P. 31125 Chihuahua, MexicoMuseum of Zoology/Laboratory Hydrobiology, Faculty of Biology, Veracruzana University, C.P. 91090 Xalapa, MexicoFaculty of Chemical Sciences, Chihuahua Autonomous University, C.P. 31125 Chihuahua, MexicoFaculty of Chemical Sciences, Chihuahua Autonomous University, C.P. 31125 Chihuahua, MexicoFaculty of Agrotechnological Sciences, Chihuahua Autonomous University, C.P. 31125 Chihuahua, MexicoMuseum of Zoology, Faculty of Biology, Veracruzana University, C.P. 91090 Xalapa, MexicoLead and chromium contamination represents one of the most serious problems in the aquatic environments. The aim of this work was to develop and validate an accurate, sensitivity, and rapid method for the simultaneous determination of Pb and Cr at trace levels in tissues and fat of marine organisms such as turtle (Chelonia mydas), shark (Rhizoprionodon terraenovae), and dolphin (Tursiops truncatus), utilizing the total reflection X-Ray fluorescence (TXRF) spectroscopy. Working solutions were prepared in 10 mL of a solution 0.005 mol·L−1 EDTA and 1 mol·L−1 HNO3. In order to correct possible instrument drifts, 20 μg·L−1 of gallium was used as internal standard (IS). The results showed that TXRF method was linear over the concentration ranges of 5.242–100 μg·L−1 for Pb and 2.363–100 μg·L−1 for Cr. Limits of detection (LOD) achieved were 1.573 and 0.709 μg·L−1 for Pb and Cr, respectively, while limits of quantification achieved were 5.242 μg·L−1 for Pb and 2.363 μg·L−1 for Cr. The validated method was accurate and precise enough for determination of these heavy metals in samples of marine organisms as indicated by acceptable values of recovery between 90–101%. In addition, a certified reference material (BCR-279, sea lettuce) and a Centrum tablet were satisfactory analyzed, and the T-test for comparison of means revealed that there were no significant differences at the 95% confidence level between the values obtained with the proposed TXRF method and the certificated values. The repeatability of the method, expressed as relative standard deviation (RSD), was 5.1% and 4%, for Pb and Cr, respectively. In addition, other features of the developed method were a low sample volume of 10 μL, and the sample frequency achieved was 20 h−1.http://dx.doi.org/10.1155/2019/8150678
spellingShingle Blanca G. Beltrán
Ibiza Martínez-Serrano
Victor Ramos-Sanchez
David Chávez-Flores
Myrna C. Nevárez-Rodríguez
Emilio A. Suárez-Domínguez
Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
Journal of Analytical Methods in Chemistry
title Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
title_full Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
title_fullStr Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
title_full_unstemmed Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
title_short Development and Validation of a New Method for Determination of Pb and Cr in Marine Organisms by Total Reflection X-Ray Fluorescence (TXRF) Spectroscopy
title_sort development and validation of a new method for determination of pb and cr in marine organisms by total reflection x ray fluorescence txrf spectroscopy
url http://dx.doi.org/10.1155/2019/8150678
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