| Literature DB >> 27320376 |
Ingrid Lima Figueiredo1, Thiago Claus1, Oscar Oliveira Santos Júnior2, Vitor Cinque Almeida1, Thiago Magon1, Jesuí Vergilio Visentainer1.
Abstract
In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures.Entities:
Keywords: Atmospheric-pressure solid analysis probe analysis; Esterification reactions; Food lipids; Sample preparation; Ultrasound
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Year: 2016 PMID: 27320376 DOI: 10.1016/j.chroma.2016.06.012
Source DB: PubMed Journal: J Chromatogr A ISSN: 0021-9673 Impact factor: 4.759