Total glycerol analysis in biodiesel samples using solid phase extraction coupled with enzymatic-spectrophotometric determination
| Autor: | Sheila Barbosa Martins, Luiz Antonio d'Avila, Cristiane Gimenes de Souza, Renan de Oliveira Muniz, Débora França de Andrade, Jéssica Nogueira da Cunha, Franck Turkovics, Eliane D'Elia, Rafael Serralvo Neto, Gláucio Gualtieri Honório, Renata Norah Chaar Pradelle |
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| Rok vydání: | 2019 |
| Předmět: |
Detection limit
chemistry.chemical_classification Biodiesel Chromatography medicine.diagnostic_test Triglyceride General Chemical Engineering 010401 analytical chemistry General Engineering Fatty acid 02 engineering and technology Repeatability 021001 nanoscience & nanotechnology 01 natural sciences 0104 chemical sciences Analytical Chemistry chemistry.chemical_compound chemistry Spectrophotometry medicine Glycerol Solid phase extraction 0210 nano-technology |
| Zdroj: | Analytical Methods. 11:767-773 |
| ISSN: | 1759-9679 1759-9660 |
| DOI: | 10.1039/c8ay02736f |
| Popis: | In this work, a method was developed for the quantification of total glycerol in biodiesel using solid phase extraction (SPE) coupled with enzymatic-spectrophotometric determination. An aminopropylsilane stationary phase was used for the separation of the main contaminants of biodiesel (monoacylglycerol (MAG), diacylglycerol (DAG), triacylglycerol (TAG) and free glycerol (FG)) from its main components, fatty acid methyl esters (FAMEs). A biodiesel sample from a high-conversion transesterification reaction was used, and the separation of contaminants was monitored by non-aqueous, reversed-phase high-performance liquid chromatography (HPLC-NARP). After SPE, the samples were analyzed by spectrophotometry using a commercial enzyme kit widely used to measure total triglyceride levels in blood. The method showed good analytical performance for linearity (R2 = 0.9919), limit of detection (9.81 × 10−4%, w/w), limit of quantification (3.24 × 10−3%, w/w), repeatability (RSD% ranged from 1.22% to 4.80%), intermediate precision and recovery (96.8% to 100%). The proposed method efficiently determined the total glycerol in biodiesel, and the paired t-test demonstrated strong correlation with the reference method (GC). |
| Databáze: | OpenAIRE |
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