2. Academic Validation
  3. Development and validation of analytical methodology by GC-FID using hexadecyl propanoate as an internal standard to determine the bovine tallow methyl esters content

Development and validation of analytical methodology by GC-FID using hexadecyl propanoate as an internal standard to determine the bovine tallow methyl esters content

  • J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Sep 1;1093-1094:134-140. doi: 10.1016/j.jchromb.2018.06.030.
Evandro Pereira 1,  Amanda Napp 2,  João V Braun 3,  Luiz A M Fontoura 3,  Marcus Seferin 4,  Jeane Ayres 5,  Rosane Ligabue 4,  Luciane M P Passaglia 6,  Marilene H Vainstein 7
Affiliations

Affiliations

  • 1 Center of Biotechnology, Universidade Federal do Rio Grande do Sul, Bento Gonçalves, 9500, CEP 91501-970 Porto Alegre, RS, Brazil. Electronic address: [email protected].
  • 2 Center of Biotechnology, Universidade Federal do Rio Grande do Sul, Bento Gonçalves, 9500, CEP 91501-970 Porto Alegre, RS, Brazil.
  • 3 Department of Process Engineering, Fundação de Ciência e Tecnologia, Campus de Cachoeirinha, Av. das Indústrias, 2270, 94930-230 Cachoeirinha, Rio Grande do Sul, Brazil.
  • 4 School of Chemistry, Pontifícia Universidade Católica do Rio Grande do Sul, 90619-900 Porto Alegre, Rio Grande do Sul, Brazil.
  • 5 School of Chemistry, Pontifícia Universidade Católica do Rio Grande do Sul, 90619-900 Porto Alegre, Rio Grande do Sul, Brazil; Institute of Environment and Natural Resources, Pontifícia Universidade Católica do Rio Grande do Sul, 90619-900 Porto Alegre, Rio Grande do Sul, Brazil.
  • 6 Departament of Genetics, Institute of Biosciences, Universidade Federal do Rio Grande do Sul, Bento Gonçalves, 9500, CEP 91500-970 Porto Alegre, RS, Brazil.
  • 7 Center of Biotechnology, Universidade Federal do Rio Grande do Sul, Bento Gonçalves, 9500, CEP 91501-970 Porto Alegre, RS, Brazil; Departament of Molecular Biology and Biotechnology, Universidade Federal do Rio Grande do Sul, Bento Gonçalves, 9500, CEP 91500-970 Porto Alegre, RS, Brazil.
PMID: 30015311 DOI: 10.1016/j.jchromb.2018.06.030
Abstract

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.

Keywords

Bovine tallow methyl esters; GC-FID; Hexadecyl propanoate; Internal standard; Method validation; Methyl heptadecanoate.

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