Fatty acids analysis by capillary electrophoresis: Fundamentals, advantages and applications.

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.

Malondialdehyde Analysis in Biological Samples by Capillary Electrophoresis: The State of Art.

Lipid peroxidation occurs when substances, such as reactive oxygen species, attack lipids. Polyunsaturated fatty acids are the main targets. Several products are formed, including primary products such as lipid hydroperoxides and secondary products such as malondialdehyde (MDA), the most used lipid peroxidation biomarker. As MDA levels are elevated in several diseases, MDA is an essential indicator for assessing pathological states. The thiobarbituric acid reactive substances assay is the most widely used method for MDA determination. However, it lacks specificity. Capillary Electrophoresis (CE) is a separation technique that has been used to quantify MDA in biological samples. This technique has advantages such as the low amount of biological sample required, absence or low volume of organic solvent, short analysis time, separation of interferents, sample preparation step with only protein precipitation, and the possibility of direct detection of the MDA, without derivatization. To our knowledge, this review article is the first to show the CE background for analyzing MDA in biological samples. Therefore, given the potential of MDA in evaluating pathological states, this article demonstrates the potential of CE to become a reference method for MDA determination in clinical analysis laboratories, which will play a significant role in diagnosing and monitoring diseases.

Determination of creatinine in urine and blood serum human samples by CZE-UV using on-column internal standard injection.

Creatinine is a well-stablished biomarker for kidney malfunctions and for normalization parameter of urinary quantitative information. Recently, metabolic studies have been discovering other functionalities for creatinine tests in human urine and blood serum. In this work we present an enhanced capillary electrophoresis (CE) based protocol for determination of creatinine. CE is a high-throughput separation technique that have been getting attention through the last decades and might be considered to be adopted as an analytical instrumentation for clinical purposes. In the proposed method, we performed a short injection program with on-column addition of internal standard. Additionally, the method allows a simultaneous screening of non-proteinogenic amino acids that could be considered for metabolomics purposes. We design a pilot study that successfully estimated the creatinine value in 100 urine samples with (2.85 ± 1.78) mg dL-1 LOD; (8.24 ± 5.93) mg dL-1 LOQ and 82.4% accuracy. Considering that serum creatinine is also included in the clinical laboratory routines for estimated Glomerular Filtration Rate dosage, the method was complementary applied to 10 blood serum samples, which resulted in a model with (0.4 ± 0.2) mg dL-1 LOD; (2.0 ± 0.6) mg dL-1 LOQ and 83.8% of accuracy. All results were in agreement with reference values. The proposed method promotes a great analytical frequency and reproducibility with enhanced specificity compared with the ongoing protocol by Jaffe's reaction, thereby proving to be useful as an alternative for creatinine exams that might help complete a diagnosis of a series of health-related issues.

Mixture design of an electrolyte system for the simultaneous separation of Cl-, SO42-, NO3-, NO2-, and HCO3- in shrimp-farming water by CZE-UV.

Shrimp is one of the most traded fishery products in the world. The shrimp-farming water ionic composition is fundamental to the growth and survival of these specimens. Therefore, this study is aimed to develop a method for the simultaneous separation of Cl-, SO42-, NO3-, NO2-, and HCO3- in this sample by capillary zone electrophoresis with UV indirect detection, without any prior sample treatment, besides dilution. The background electrolyte (BGE) was composed of CrO42- (60 mmol L-1), cetyltrimethylammonium bromide (CTAB, 2.5 mmol L-1), acetonitrile (0.875% (v/v)), and methanol (2.625% (v/v)). The mixture design optimized the BGE composition. Acetonitrile and methanol changed the degree of solvation of the anions, which decreased the radius, a phenomenon proven by calculating the radius of anions in all the conditions of the mixture design. The optimized and validated method allowed the simultaneous determination of the five above-mentioned anions in 10 min.

Short-End Injection Capillary Electrophoresis and Multivariate Analysis for Simultaneous Determination of Heavy Metals in Passiflora incarnata Tea.

An ultra-fast method for the simultaneous determination of heavy metals in Passiflora incarnata tea by capillary electrophoresis (CE) using a short-end injection combined with multivariate analysis was proposed. Separation was conducted by hydrodynamic injection (5 s at 0.5 psi) using the short-end injection procedure in a fused uncoated silica capillary (50 cm total length, 10.2 cm effective length, 50 µm i.d.) with separation time less than 2 min. An indirect UV detection at 214 nm was employed by using imidazole as a chromophore. The buffer used was 6 mmol/L hydroxybutyric acid (HIBA). The optimum conditions by full factorial with a central point were achieved by 18-crown-6 concentration (23.3 mmol L−1), voltage (+11.4 kV), methanol concentration (3.8%), and temperature (20 °C). The method showed good linearity (R2 > 0.998) for both Cd and Pb, inter-day precision of less than 14.49%, and an adequate limit of quantification only for Cd (LOQ < 0.5 µg mL−1 for Cd) based on the US Pharmacopeial Convention limit requirements for elemental impurities. After method validation, the method was applied to Passiflora incarnata tea samples from a local market. Furthermore, the developed method showed great potential for the determination of metals in other samples with proper sample preparation procedures.

Determination of purity and anionic exchange efficiency of amino acid ionic liquids synthesis by multiple-injection capillary zone electrophoresis.

The purity of ionic liquids (IL) is important for its performance, so the methods able to quantify low concentration impurities are necessaries. Therefore, this paper aims to determine the purity and the anionic exchange efficiency for the preparation of amino acids ionic liquids (AAIL). For this, a Multiple-Injection Capillary Zone Electrophoresis (MICZE) method with direct UV detection was developed and optimized for iodide (I-) determination as impurity of AAIL synthesis, comparing this method with traditional injection modes. Furthermore, this paper aims to demonstrate the use of factorial design methods for the optimization of MICZE method. The method optimization allowed five consecutives I- injections of sample in a single run, with analysis time of less than 3 min, showing a larger analytical frequency, counting with 31 injections per hour. It was possible to determine the high purity of the prepared and analyzed AAIL, ranging from 89% to 95% and its overall ionic exchange yield varying from 55% to 87%.

Nb2O5 supported in mixed oxides catalyzed mineralization process of methylene blue.

Heterogeneous photocatalysis has become a significant green technology for water treatment. The application of Nb2O5 catalyst for the photodegradation of contaminants has merged as an important tool to this process. Furthermore, it is known that catalytic phases supported on metal oxides are an alternative method for enhancing its activity. In this work, supported Nb2O5 on mixed oxides as catalyst was applied to degrade methylene blue dye, leading to almost 100% of dye degradation without the need of any additives, after only three hours of sunlight exposure. The effect of catalyst concentration, exposure time and light source were investigated. The best catalyst activity was found at 1.5 g L-1 and for higher catalyst concentrations the degradation was kept constant. Plausible intermediates of this degradation process were observed and characterized by NMR, LC/MS and CZE techniques. After degradation, the catalyst was recovered and could be further re-applied in other three reaction cycles without significant loss of catalytic activity.