Development of a method for the determination of polyamines including N-acetylated forms in human saliva via benzoylation and gas chromatography-mass spectrometry
[EN]A simple method for the determination of polyamines and their N -acetylated forms was developed us- ing benzoyl chloride as derivatization reagent, and 1,6-diaminohexane as internal standard, followed by liquid-liquid extraction with ethyl acetate. The organic extract was injected in a gas chrom...
| Autores: | , , , |
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| Tipo de recurso: | artículo |
| Estado: | Versión publicada |
| Fecha de publicación: | 2021 |
| País: | España |
| Institución: | Universidad de Salamanca (USAL) |
| Repositorio: | GREDOS. Repositorio Institucional de la Universidad de Salamanca |
| OAI Identifier: | oai:gredos.usal.es:10366/154874 |
| Acceso en línea: | http://hdl.handle.net/10366/154874 |
| Access Level: | acceso abierto |
| Palabra clave: | Polyamines Saliva samples Benzoyl chloride derivatization Gas chromatography-mass spectrometry |
| Sumario: | [EN]A simple method for the determination of polyamines and their N -acetylated forms was developed us- ing benzoyl chloride as derivatization reagent, and 1,6-diaminohexane as internal standard, followed by liquid-liquid extraction with ethyl acetate. The organic extract was injected in a gas chromatograph using a programmed temperature vaporizer and the determination and quantification was performed with a quadrupole mass spectrometer. There was no matrix effect with the proposed method, so internal cali- bration was used to quantify the corresponding derivatives. Good linear responses were obtained in the range from the limits of detection to 500 μg L −1 (50 μg L −1 for spermidine), with correlation coefficients varying from 0.9591 to 0.9968. The limits of quantification (S/ N = 10) ranged 1.0 –8.3 μg L −1 . Recoveries were found between 82 –117%, showing the good accuracy of the proposed method. Intra- and inter-day precision assays, expressed as relative standard deviation (RSD) were evaluated at two different concen- tration levels (low and high), showing values in the range of 2.4 –6.1% and 5.2 –9.0% for repeatability and reproducibility, respectively (6.9 –9.7% and 14.1 –14.6% for spermidine). Successfuldetermination of the studied polyamines and their N -acetylated forms was performed on the saliva of 17 volunteers. |
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