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Development and validation of analytical methodology by GC-FID using hexadecyl propanoate as an internal standard to determine the bovine tallow methyl esters content
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-06-20 , DOI: 10.1016/j.jchromb.2018.06.030
Evandro Pereira , Amanda Napp , João V. Braun , Luiz A.M. Fontoura , Marcus Seferin , Jeane Ayres , Rosane Ligabue , Luciane M.P. Passaglia , Marilene H. Vainstein

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.



中文翻译:

通过GC-FID开发和验证GC-FID分析法,使用丙酸十六烷基酯作为内标测定牛脂牛油酯含量

为了确定生物柴油的脂肪酸甲酯(FAME)含量,制定了EN 14103:2003和EN 14103:2011。生物柴油的内标(IS)分别包括十七烷酸甲酯(MHD)和壬二酸甲酯(MND)。但是,由于这些IS也存在于牛脂甲酯(BTME)或重叠峰中,因此效率不高。这项工作提出了一种通过使用丙酸十六烷基酯(HDP)作为IS的改进的BTME测定方法。为此,开发并验证了气相色谱-火焰电离检测器(GC-FID)的分析方法,其中HDP证明了对于椰子和大豆甲酯和BTME而言,在峰C16:1和C18:0之间的保留时间具有选择性,以及在拆分模式30:1下BTME的分辨率> 1.5。使用HDP作为IS来确定BTME含量的真实性在统计学上等同于原假设统计检验的95%置信区间,即使与EN 14103定义的IS浓度相比仅使用了20%的HDP: 2003和EN 14103:2011。这使得用1 g HDP进行的生物柴油分析可以进行五次以上。此外,开发的方法使我们能够将分析时间减少21.6%,而不会影响峰的积分(C6:0至C24:1)。关于重复性和中间精度测试,达到RSD(%)≤2%的结果。此外,已证明开发的方法是可靠的。HDP是生物柴油合成所用原料中不存在的长链脂肪醇酯。它代表了良好IS的所有特征,

更新日期:2018-06-20
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