Abstract:Decaffeinated coffee accounts for 10 percent of coffee sales in the world; it is preferred by consumers that do not wish or are sensitive to caffeine effects. This article presents an analytical comparison of capillary electrophoresis (CE) and high performance liquid chromatography (HPLC) methods for residual caffeine quantification in decaffeinated coffee in terms of validation parameters, costs, analysis time, composition and treatment of the residues generated, and caffeine quantification in 20 commercial s… Show more
“…Comparing the HPLC and CE methods developed for evaluation of BF of T. patula , CE was more efficient, being almost four times faster. In addition, in the CE method, organic solvents are not used to separate the analytes, and the volume of electrolytic solution used for analyses is small, making the technique less costly and polluting [ 39 – 41 ].…”
The crude acetone extract (CAE) of defatted inflorescences of Tagetes patula was partitioned into five semipurified fractions: n-hexane (HF), dichloromethane (DF), ethyl acetate (EAF), n-butanol (BF), and aqueous (AQF). BF was fractionated by reversed-phase polyamide column chromatography, obtaining 34 subfractions, which were subjected to HSCCC, where patuletin and patulitrin were isolated. CAE and the fractions BF, EAF, DF, and AQF were analyzed by LC-DAD-MS, and patuletin and patulitrin were determined as the major substances in EAF and BF, respectively. BF was also analyzed by HPLC and capillary electrophoresis (CE), and patulitrin was again determined to be the main substance in this fraction. CAE and the semipurified fractions (750, 500, 300, 100, and 50 mg/L) were assayed for larvicidal activity against Aedes aegypti, with mortality rate expressed as percentage. All fractions except AQF showed insecticidal activity after 24 h exposure of larvae to the highest concentration. However, EAF showed the highest activity with more than 50% reduction in larval population at 50 mg/L. The insecticidal activity observed with EAF might have been due to the higher concentration of patuletin present in this fraction.
“…Comparing the HPLC and CE methods developed for evaluation of BF of T. patula , CE was more efficient, being almost four times faster. In addition, in the CE method, organic solvents are not used to separate the analytes, and the volume of electrolytic solution used for analyses is small, making the technique less costly and polluting [ 39 – 41 ].…”
The crude acetone extract (CAE) of defatted inflorescences of Tagetes patula was partitioned into five semipurified fractions: n-hexane (HF), dichloromethane (DF), ethyl acetate (EAF), n-butanol (BF), and aqueous (AQF). BF was fractionated by reversed-phase polyamide column chromatography, obtaining 34 subfractions, which were subjected to HSCCC, where patuletin and patulitrin were isolated. CAE and the fractions BF, EAF, DF, and AQF were analyzed by LC-DAD-MS, and patuletin and patulitrin were determined as the major substances in EAF and BF, respectively. BF was also analyzed by HPLC and capillary electrophoresis (CE), and patulitrin was again determined to be the main substance in this fraction. CAE and the semipurified fractions (750, 500, 300, 100, and 50 mg/L) were assayed for larvicidal activity against Aedes aegypti, with mortality rate expressed as percentage. All fractions except AQF showed insecticidal activity after 24 h exposure of larvae to the highest concentration. However, EAF showed the highest activity with more than 50% reduction in larval population at 50 mg/L. The insecticidal activity observed with EAF might have been due to the higher concentration of patuletin present in this fraction.
“…In the last five years, CE has been applied in many fields including the analysis of plant materials [ 86 ]. While HPLC did provide lower values of LOD for the determination of caffeine in decaffeinated coffee than CE, the latter was 30% faster, had lower cost of reagents, and generated smaller volumes of residues [ 137 ]. In a similar experiment, a fast hydrodynamic injection (50 mBar, 7 s) was applied in the analysis of caffeine in commercial decaffeinated coffee using a 48 cm × 50 μ m fused-silica capillary [ 138 ].…”
Section: Methods For Characterization and Quantification Of Bioactmentioning
Production of coffee beans is an important lifeline for the economy of several countries in Latin America, Africa, and Asia. The brew from this well sought for cash crop is readily consumed due to its good sensory qualities owing to the presence of many micronutrients. Some of these chemical compounds possess biological activities, including antiproliferative, antioxidant, and antimicrobial effects. Four representative groups of these micronutrients, namely, caffeine, chlorogenic acid, diterpenes, and trigonelline, play key roles in these bioactive effects of coffee. In order to guarantee the quality of coffee products and to protect consumer interest and safeguard their well-being, it is extremely important to employ sensitive and accurate analytical methods in the characterization and quantitative determination of these bioactive constituents. This review aims to present recent applications in this regard.
“…Both caffeine and taurine content are usually determined by high-performance liquid chromatography with diode array detector (HPLC-DAD) (Bizzotto et al, 2013;Chirita Tampu et al, 2018;Paula Lima & Farah, 2019;Rai et al, 2016) and capillary electrophoresis, mainly zone or micellar electrokinetic chromatography (MEKC) with diode array detector (DAD), is also often employed. However, taurine does not absorb light in the UV -VOS region, being detected indirectly, either by DAD, or by laser -induced fluorescence, amperometric and conductometric detectors (Rai et al, 2016;Sawabe et al, 2008;Vochyánová et al, 2014;Zinellu et al, 2009).…”
The objective of this study was to develop, optimize and validate a fast and reliable method for the simultaneous determination of caffeine and taurine contents by micellar electrokinetic chromatography with diode array detector, using direct and indirect detection concomitantly. Multivariate statistical techniques were used as a central composite design and the simultaneous optimization method of responses of Derringer and Suich were used for optimization. The method was applied in the analysis of 73 samples of energy drinks commercialized in Brazil. The optimized method employed a capillary tube with an extended bulb of 50 µm i.d. x 72 cm total length, an electrolyte containing 16.20 mmol.L-1 of benzoic acid and 39.90 mmol.L-1 of SDS, a pH value of 7.26, + 30 kV voltage, direct detection of caffeine at 274 nm and indirect detection of taurine at 230 nm. Validation parameters have demonstrated the reliability and applicability of this method. Ot was found that more than 50% of the samples were out of the legal limits determined by the Brazilian government regarding the taurine content and 68 % contained caffeine below the value declared on the label. Therefore, the need for greater control concerning the composition of these drinks exists.
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