Development and validation of analytical methodology by GC-FID using hexadecyl propanoate as an internal standard to determine the bovine tallow methyl esters content
| Autor: | Marcus Seferin, Luciane Maria Pereira Passaglia, Amanda P. Napp, João Vitor Braun, Luiz Antonio Mazzini Fontoura, Marilene Henning Vainstein, Jeane Ayres, Evandro Pereira, Rosane Angélica Ligabue |
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| Rok vydání: | 2018 |
| Předmět: |
Chromatography
Gas Resolution (mass spectrometry) 020209 energy Clinical Biochemistry Fatty alcohol 02 engineering and technology 01 natural sciences Biochemistry Analytical Chemistry Fats chemistry.chemical_compound Tallow 0202 electrical engineering electronic engineering information engineering Animals Fatty acid methyl ester Flame Ionization Biodiesel Chromatography Fatty Acids 010401 analytical chemistry Reproducibility of Results Cell Biology General Medicine Repeatability Reference Standards 0104 chemical sciences chemistry Biofuels Cattle Propionates Selectivity Decanoic Acids Retention time |
| Zdroj: | Journal of Chromatography B. :134-140 |
| ISSN: | 1570-0232 |
| Popis: | EN 14103:2003 and EN 14103:2011 were developed in order to determine fatty acid methyl ester (FAME) content of biodiesel. The internal standards (IS) of biodiesel include methyl heptadecanoate (MHD) and methyl nonadecanoate (MND), respectively. However, since these ISs are also present in bovine tallow methyl esters (BTME) or overlapping peaks, they have not been efficient. This work proposes an improved BTME determination method by using hexadecyl propanoate (HDP) as an IS. For this purpose, an analytical methodology by Gas Chromatography-Flame Ionization Detector (GC-FID) was developed and validated, where HDP demonstrated selectivity in retention time between peaks C16:1 and C18:0 for coconut and soybeans methyl esters and BTME, as well as resolution >1.5 for the BTME in split mode 30:1. Trueness in the determination of BTME content using the HDP as an IS was statistically equivalent to confidence interval of 95% for the null hypothesis statistic test, even when only 20% of the HDP was utilized in comparison with the IS concentrations defined by EN 14103:2003 and EN 14103:2011. This allowed the biodiesel analysis to be performed five times more with 1 g of HDP. Furthermore, the method developed enabled us to reduce the analysis time by 21.6%, without prejudice to the integration of peaks (C6:0 to C24:1). Regarding the repeatability and intermediate precision tests, results of RSD (%) ≤ 2% were reached. Additionally, the method developed has proved to be robust. HDP is a long-chain fatty alcohol ester absent from feedstocks used in biodiesel synthesis. It presents all of the characteristics for a good IS, ideal for application via internal standardization method, as recommended by EN 14103. |
| Databáze: | OpenAIRE |
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