Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy
Selenium (Se) is a trace element used by multiple enzymes. In ruminants, Se present in food is released to ruminal fluid allowing its absorption in the small intestine. Se release may be analysed by hydride generation atomic absorption spectroscopy (HG-AAS). According to the Association Official of...
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| Format: | info:ar-repo/semantics/artículo |
| Language: | Inglés |
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Ediciones INTA
2021
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| Online Access: | http://hdl.handle.net/20.500.12123/9227 |
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| author | Brambilla, Emilio Cesar Cseh, Susana Beatriz Fernandez, Eduardo Luján San Martino, Silvina |
| author_browse | Brambilla, Emilio Cesar Cseh, Susana Beatriz Fernandez, Eduardo Luján San Martino, Silvina |
| author_facet | Brambilla, Emilio Cesar Cseh, Susana Beatriz Fernandez, Eduardo Luján San Martino, Silvina |
| author_sort | Brambilla, Emilio Cesar |
| collection | INTA Digital |
| description | Selenium (Se) is a trace element used by multiple enzymes. In ruminants, Se present in food is released to ruminal fluid allowing its absorption in the small intestine. Se release may be analysed by hydride generation atomic absorption spectroscopy (HG-AAS). According to the Association Official of Analytical Chemists (AOAC), analysing the methodological performances is important to support the results of a methodology. The aim of this study was to develop and verify the analytical methodology of Se determination in ruminal fluid by HG-AAS. According to the AOAC guide, the parameters to be analyzed, and their respective acceptance criteria (AC) are: applicable range (AC: 0.220 - 9.68 µg/l), bias (AC: 70-125%), precision by repeatability (RSDr%) (AC: < 21%), intermediate precision (RSDip%) (AC: < 21%), recovery (AC: 80-110%), limit of detection (LOD) (AC: < 0.22 µg/l), and relative uncertainty (AC: <15%). The technique used is based on a wet digestion of ruminal fluid with HClO4 , H2 SO4 and HNO3 concentrated at temperatures ranging from 120°C to 180°C. Then the digest was pre-reduced in HCl at 50 % and was quantified in the HG-AAS. The results obtained were: LOD 0.196 µg/l, bias 96.8% (1.25 µg/l); 98.3% (2.50 µg/l); 94.8% (5.00 µg/l), precision by repeatability 8.61% (3.28 µg/l); 8.90 % (3.52 µg/l); 9.80% (1.85 µg/l), intermediate precision RDSip 10.2%, recovery 109.2% (10 µg/l); 96.7% (25 µg/l); 96.8% (50 µg/l) and applicable range 0.196-62.5 µg/l. The values obtained are within the requirements stated by the AC. |
| format | info:ar-repo/semantics/artículo |
| id | INTA9227 |
| institution | Instituto Nacional de Tecnología Agropecuaria (INTA -Argentina) |
| language | Inglés |
| publishDate | 2021 |
| publishDateRange | 2021 |
| publishDateSort | 2021 |
| publisher | Ediciones INTA |
| publisherStr | Ediciones INTA |
| record_format | dspace |
| spelling | INTA92272024-10-31T16:08:26Z Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy Brambilla, Emilio Cesar Cseh, Susana Beatriz Fernandez, Eduardo Luján San Martino, Silvina Ganado Bovino Selenio Oligoelementos Espectrometría Cattle Selenium Trace Elements Spectrometry Selenium (Se) is a trace element used by multiple enzymes. In ruminants, Se present in food is released to ruminal fluid allowing its absorption in the small intestine. Se release may be analysed by hydride generation atomic absorption spectroscopy (HG-AAS). According to the Association Official of Analytical Chemists (AOAC), analysing the methodological performances is important to support the results of a methodology. The aim of this study was to develop and verify the analytical methodology of Se determination in ruminal fluid by HG-AAS. According to the AOAC guide, the parameters to be analyzed, and their respective acceptance criteria (AC) are: applicable range (AC: 0.220 - 9.68 µg/l), bias (AC: 70-125%), precision by repeatability (RSDr%) (AC: < 21%), intermediate precision (RSDip%) (AC: < 21%), recovery (AC: 80-110%), limit of detection (LOD) (AC: < 0.22 µg/l), and relative uncertainty (AC: <15%). The technique used is based on a wet digestion of ruminal fluid with HClO4 , H2 SO4 and HNO3 concentrated at temperatures ranging from 120°C to 180°C. Then the digest was pre-reduced in HCl at 50 % and was quantified in the HG-AAS. The results obtained were: LOD 0.196 µg/l, bias 96.8% (1.25 µg/l); 98.3% (2.50 µg/l); 94.8% (5.00 µg/l), precision by repeatability 8.61% (3.28 µg/l); 8.90 % (3.52 µg/l); 9.80% (1.85 µg/l), intermediate precision RDSip 10.2%, recovery 109.2% (10 µg/l); 96.7% (25 µg/l); 96.8% (50 µg/l) and applicable range 0.196-62.5 µg/l. The values obtained are within the requirements stated by the AC. El selenio (Se) es un elemento traza utilizado por múltiples enzimas. En rumiantes, el Se de los alimentos es liberado hacia el licor ruminal y esto permite su absorción en el intestino delgado. El Se liberado puede ser analizado por espectrofotometría de absorción atómica con plataforma de hidruros (HG-AAS) De acuerdo con la asociación oficial de química analítica (AOAC) analizar la performance metodológica es importante para respaldar los resultados de una metodología. El objetivo de este estudio fue el desarrollo y verificación de la metodología analítica de la determinación de Se en fluido ruminal mediante un HG-AAS. De acuerdo con la guía de la AOAC, los parámetros para analizar para esto, y sus respectivos criterios de aceptación (CA), son: rango aplicable (CA: 0,22-9,68 µg/l), bias (CA: 70-125%), precisión por repetibilidad (CA: RSDr <21%), precisión intermedia (CA: RSDR <21%), recuperación (CA: 80-110%) y límite de detección (LOD) (CA: <0,22 µg/l), incertidumbre relativa expandida (CA: <15%). La técnica que se utilizó se basó en una digestión húmeda del fluido ruminal con HClO4 (c), H2 SO4 (c) y HNO3 (c) a temperaturas que van de los 120 o C a 180 o C. Luego se realiza una prerreducción del equis con HCl al 50% y se cuantificó en el HG-AAS. Los resultados obtenidos fueron los siguientes: LOD 0,196 µg/l, Bias 96,8% (1,25 µg/l); 98,3% (2,50 µg/l); 94,8% (5,00 µg/l), equisite por repetibilidad 8,61% (3,28 µg/l); 8,90% (3,52 µg/l); 9,80% (1,85 µg/l), equisite intermedia RDSR 10,2%, recuperación 109, 2% (10 µg/l); 96,7% (25 µg/l); 96,8% (50 µg/l) y rango equisites 0.196-62,5 µg/l. Los valores obtenidos están dentro de los equisites mínimos indicados por los CA. EEA Balcarce Fil: Brambilla, Emilio Cesar. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Balcarce; Argentina Fil: Cseh, Susana Beatriz. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Balcarce; Argentina Fil: Fernandez, Eduardo Luján. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Balcarce; Argentina Fil: San Martino, Silvina. Universidad Nacional de Mar del Plata. Facultad de Ciencias Agrarias. Departamento de Introducción a las Ciencias Agrarias. Estadística y Diseño Experimental; Argentina 2021-04-29T17:31:31Z 2021-04-29T17:31:31Z 2021-04 info:ar-repo/semantics/artículo info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion http://hdl.handle.net/20.500.12123/9227 0325-8718 1669-2314 eng info:eu-repo/semantics/openAccess http://creativecommons.org/licenses/by-nc-sa/4.0/ Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0) application/pdf Ediciones INTA RIA 47 (1) : 104-109 (Abril 2021) |
| spellingShingle | Ganado Bovino Selenio Oligoelementos Espectrometría Cattle Selenium Trace Elements Spectrometry Brambilla, Emilio Cesar Cseh, Susana Beatriz Fernandez, Eduardo Luján San Martino, Silvina Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title | Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title_full | Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title_fullStr | Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title_full_unstemmed | Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title_short | Methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| title_sort | methodological performance of selenium determination in ruminal fluid by hydride generation atomic absorption spectroscopy |
| topic | Ganado Bovino Selenio Oligoelementos Espectrometría Cattle Selenium Trace Elements Spectrometry |
| url | http://hdl.handle.net/20.500.12123/9227 |
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