The advent of policies that incentivize or require alternative diesel fuels has increased the demand for the development of fast analytical methods aiming for the quality control of these fuels. This ...study approached an alternative method for the determination of biodiesel acidity employing capillary zone electrophoresis based on free fatty acids screening and quantification. Sample preparation comprised vortex‐assisted liquid‐liquid extraction of free fatty acids and was a crucial step for analysis. It was studied through a 32 full factorial design considering sample mass and the stirring time. Then, solvent suitability was evaluated univariately. The free fatty acid screening was carried out employing a capillary zone electrophoresis method able to separate C16:0, C18:0, C18:1 n‐9, C18:2 n‐6, and C18:3 n‐3, major fatty acids in a variety of vegetable oils used for biodiesel synthesis. In addition to the straightforward sample preparation protocol, the running time of the developed method was only 12 min. Moreover, ultraviolet absorption indirect detection of analytes was approached to avoid analytes derivatization, considering the lack of chromophore groups in saturated fatty acids. Statistical tests did not evidence any significant differences in the biodiesel acidity determination expressed in percentage of free fatty acids when comparing the proposed capillary zone electrophoresis method and the traditional potentiometric titration approach within the 95% confidence interval, which demonstrates the suitability of this alternative method for the biodiesel quality control in routine.
Fatty acids determination is of paramount importance for quality control and suitable labeling of edible oils, required by regulatory agencies in several countries, and fast methods for this ...determination are worldly desired. This review article aimed to explore the available analytical methods for vegetable and marine oils analyses employing CE, which can be a straightforward and faster alternative than GC methods for fatty acid determination, considering some purposes. CE usually offers the possibility of a rapid analysis with a simple preparation of the sample, without requiring specific columns, which are inherent advantages of the technique. Instrumental conditions and the key points about fatty acids determination employing the technique are highlighted, and the main challenges and perspectives are also approached. Potential use of CE for edible oil analyses has been demonstrated for research and routine, which can be of interest for industries, regulatory agencies, and edible oil researchers. Therefore, we have explored the analytical approaches described in the last decades, intending to spread the interest of CE methods for fatty acid monitoring, label accuracy assessment, and food authenticity evaluation of edible oils.
A review taking into account the literature reports covering 20 years of fatty acid analysis by capillary electrophoresis is presented. This paper describes the evolution of fatty acid analysis using ...different CE modes such as capillary zone electrophoresis, non-aqueous capillary electrophoresis, micellar electrokinetic capillary chromatography and microemulsion electrokinetic chromatography employing different detection systems, such as ultraviolet-visible, capacitively coupled contactless conductivity, laser-induced fluorescence and mass spectrometry. In summary, the present review signals that CE seems to be an interesting analytical separation technique that is very useful for screening analysis or quantification of the usual fatty acids present in different matrices, offering short analysis times and a simple sample preparation step as inherent advantages in comparison with the classical methodology, making it a separation technique that is very attractive for quality control in industry and government agencies.
Ruminant milk is the lead source of conjugated linoleic acid (CLA) in the human diet, with cis-9, trans-11 CLA being the major among all. Small amounts of trans-10, cis-12 CLA are also found in ...synthetic supplements. Since both isomers are biologically active with potential health benefits, there is great interest in quantifying them for quality control routines. An alternative method for the analysis of the aforementioned CLAs by fast gas chromatography (GC) is discussed in the present study. The fatty acid methyl ester mixture obtained by alkaline catalysis was injected into a GC equipped with a flame ionization detector (FID) and fitted with an ionic liquid SLB-IL111 chromatographic column (15 m × 0.10 mm × 0.08 µm). Separation was achieved in less than 5 min using a 168 °C isotherm run. Both CLA isomers were quantified by using of single point standard addition statistical approach. Results were contested to those obtained using the recommended 100 m long CP-Sil88 capillary column and none evidence of significant differences was found within 95% confidence interval. Therefore, the proposed method could be valuable to focused regulatory routines of large numbers of samples with greater analytical frequency.
The precursor compounds related to the bitterness of beer are called α‐acids. These compounds are extracted from the hop, which is an important ingredient in the brewing process. These compounds were ...analyzed by capillary electrophoresis. The electrophoretic method used 160 mmol/L of ammonium carbonate (pH 9) as BGE (background electrolyte), a voltage of +20 kV in a capillary with 50 μm of internal diameter and with a 62.5 cm of total length (54 cm effective). The samples were injected in hydrodynamic mode applying a pressure of 25 mbar for 5 s and the analytes were detected at 230 nm. A hydromethanolic extraction during 3 h was considered as the optimum condition for the sample preparation using MeOH/H2O 80:20 v/v as the extract solution. From the optimized conditions the electropherograms were evaluated for their use as input for chemometric modeling. Preprocessing investigation for electrophoretic data taking into account the alignment, denoising and baseline correction, and variable selection were considered before the chemometric modeling using principal component analysis (PCA). The electrophoretic data were systematically evaluated to find the optimum conditions to modeling. A PCA analysis for all tests was carried out using different preprocessing methods and, an explained variance higher than 90% was achieved in all of them. The optimized chemometric method worked with aligned and meancentered data. From this approach, a simple and efficient method to classify hop samples with high and low α‐acids content without the use of analytical standards was established from a simple electrophoretic analysis.
•A rapid CZE method for the analysis ofcitrate, phosphate and sulfitewas developed.•The analytes were separated in less than 3.5 min.•Seafood samples were analyzed by the validated CZE ...method.•In-house method validation was performed to confirm the fitness-for-purpose.
Since seafood is susceptible to decomposition, additives may be used to maintain its quality. However, some additives may be improperly used to disguise spoilage, thus resulting in food fraud. Market growth demands faster and more reliable quality control tools that incorporate the most common additives in a single analysis. This study developed a rapid analytical method for the determination of citrate, phosphate and sulfite in seafood by capillary zone electrophoresis with indirect UV–Vis detection. Electrophoretic separation was achieved in less than 3.5 min. The background electrolyte consisted of 20 mmol L−1 of benzenesulfonic acid and 45 mmol L−1 of aminocaproic acid. After validation, the method was applied for 24 seafood real samples. Citrate was found in five samples. Four samples presented higher phosphate and sulfite concentrations than those permitted by Brazilian legislation. Good analytical performance indicates that the method is a viable alternative for food control in routine analysis.
This review covers the know‐how of the Grupo de Química Analítica e Quimiometria regarding the analysis of fatty acids by capillary electrophoresis acquired over its 20 years of existence. Therefore, ...the fundamentals, advantages, and applications of this technique for analyzing different fatty acids in samples such as food, oils, cosmetics, and biological matrices are presented and discussed. Capillary electrophoresis is, thus, shown as an interesting and valuable separation technique for the target analysis of these analytes as an alternative to the gas chromatography coupled to flame ionization detection, as it offers advantages over the latter such as low analysis times, low sample and reagent consumption, the use of a nondedicated column, and simpler sample preparation. In addition, the methods shown in this literature review can be useful for quality control, adulteration, and health‐related research by regulatory agencies.
A validated sub minute capillary zone electrophoresis method with direct ultraviolet absorption detection for simultaneous determination of isoniazid and rifampicin in fixed‐dose combination tablets ...was developed. Background electrolyte was defined based on the analytes effective mobility curve and it was composed by 20 mmol/L of sodium carbonate/sodium bicarbonate at pH 10.2. A careful validation procedure considering the main figures of merit was performed. Regression models were satisfactory for isoniazid and rifampicin, showing no lack of fit within 95% significance interval. Interday and intraday precision were evaluated in standard and sample and slight relative standard deviations were achieved for concentration, area, and migration time. Recovery values for accuracy in two levels were 99.97 and 90.08% for isoniazid and 95.45 and 95.12% for rifampicin. The limits of detection for isoniazid and rifampicin were 0.22 and 0.34 mg/L, respectively, and the limits of quantification were 0.74 and 1.13 mg/L, respectively. Method selectivity was verified by injecting diluent, background electrolyte, a standard mixture, and a sample, confirming no interferent peaks. The method proved to be simple, environmentally friendly, sensitive, and was successfully applied for simultaneous quantification of isoniazid and rifampicin in fixed‐dose combination tablets.
Capillary electrophoresis (CE) is a technique that may offer high-resolution separations in complex matrices with a short analysis time. It generally employs straightforward sample preparation ...protocols and requires low amounts of sample and reagents, which follows the green chemistry concept. This review presents several methods developed within the 2010s decade, aiming simpler and faster food analyses in the determination of lipids applying CE. It summarizes sample preparation protocols, background electrolyte, and instrumental conditions optimized in each method. Different CE modes and detection systems are discussed, as well as figures of merit of the developed analytical methods. Moreover, it approaches significant challenges involved with lipid assay by CE and opportunities for innovation in the lipid research.
In the present work, we describe the preparation of ten amino acid ionic liquids (AAILs) formed from ammonium salts as cations, derivatives of glycerol, and natural amino acids as anions. All of them ...are viscous oils, colorless or pale yellow, and hygroscopic at room temperature. They have appreciable solubility in many protic and aprotic polar solvents. The AAILs were used as catalysts in a Morita-Baylis-Hillman (MBH) reaction. The ionic liquids derivative from l-proline and l-histidine demonstrated the ability to catalyze the reaction between methyl vinyl ketone and aromatic aldehydes differently substituted in the absence of an additional co-catalyst under organic solvent-free conditions. The AAIL derivatives from l-valine, l-leucine, and l-tyrosine catalyzed the MBH reaction only in the presence of imidazole. The MBH adducts were obtained in moderate to good yields. Although the catalytic site in the ILs was in its enantiomerically pure form, all the MBH adducts were obtained in their racemic form.
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