RESUMO
Colorimetric determination of proteins in serum is proposed based on the biuret method and replacing ultraviolet-visible spectrometric (UV-Vis) detection with a simple and affordable smartphone digital image colorimetric (SDIC) method. Optimum SDIC conditions were found as a detection wavelength of 555 nm, a region of interest of 1600 px2, and 9.0 cm between the detection camera and sample solution. Under the optimum conditions, the coefficient of determination was 0.9982 within a linear dynamic range of 0.022 to 0.35 g dL-1. The precision of the method based on the percent relative standard deviation was below 5%. The limit of detection and limit of quantitation were found to be 0.007 and 0.022 g dL-1 respectively, which were sufficient for the quantification of the total protein, albumin, and globulin in serum. The method was validated with an independent experiment using a UV-Vis method and both methods showed good statistical agreement, indicating the accuracy of the proposed SDIC method.
Assuntos
Colorimetria , Smartphone , Colorimetria/métodos , Limite de Detecção , Proteínas Sanguíneas , Espectrofotometria UltravioletaRESUMO
Simple, inexpensive and accurate analytical methods are in high demand. Dispersive solid-phase microextraction (DSPME) was used in combination with smartphone digital image colorimetry (SDIC) to determine boron in nuts as an approach replacing existing costly alternatives. A colorimetric box was designed to capture images of standards and sample solutions. ImageJ software was used to link pixel intensity to the analyte concentration. Under optimum extraction and detection conditions, linear calibration graphs were obtained with coefficients of determination (R2) above 0.9955. Percentage relative standard deviations (%RSD) were below 6.8 %. The limits of detection (LOD) ranged between 0.07 and 0.11 µg mL-1 (1.8 to 2.8 µg g-1), which were sufficient for detection of boron in nut samples (i.e., almond, ivory, peanut and walnut), with percentage relative recoveries (%RR) between 92.0 and 106.0 %.
Assuntos
Colorimetria , Microextração em Fase Líquida , Colorimetria/métodos , Boro , Smartphone , Microextração em Fase Líquida/métodos , Microextração em Fase Sólida/métodos , Limite de DetecçãoRESUMO
Objectives: This study aims to present a method for the determination of the aluminum in antiperspirant products (APPs) by chelating it with quercetin before its detection by smartphone digital image colorimetry (SDIC). Materials and Methods: Samples were prepared by closed-vessel acid digestion in PTFE cups. This was followed by complexation of aluminum in the sample solution using quercetin as a chelating agent. Sample solutions were transferred into a quartz ultraviolet/visible detection microcuvette for detection in a homemade colorimetric box designed for capturing images of the yellow complex with a smartphone camera. The pixel intensity of the images was converted to numbers for quantitation using ImageJ software for a personal computer. An independent study using high-performance liquid chromatography-diode-array detection was conducted to check the accuracy of the proposed method. Results: Optimum SDIC conditions included a Samsung C9 smartphone as the detection camera, a cropped region of interest of 6400 px2, and the side position of the colorimetric box were selected for capturing the images of the sample solutions placed 10.0 cm from the detection camera, whereas optimum complexation conditions were found to be as sample pH of 5.5, sample volume of 3.0 mL, complexation time of 1.0 min and a ligand concentration of 0.28 mmol L-1. Analytical performance of the method included a limit of detection of 0.5 µmol L-1 and a coefficient of determination (R2) of the calibration graph of 0.9981. Conclusion: The proposed method was successfully applied for the determination of aluminum in APPs with percentage recoveries ranging from 80.0 to 109.6%.
RESUMO
Dispersive liquid-liquid microextraction (DLLME) was combined with high-performance liquid chromatography-diode-array detector (HPLC-DAD) for the extraction and quantitation of three major capsaicinoids (i.e. capsaicin, dihydrocapsaicin and nordihydrocapsaicin) from pepper (Capsicum annuum L.). Chloroform (extraction solvent, 100 µL), acetonitrile (disperser solvent, 1250 µL) and 30 s extraction time were found optimum. The analytes were back-extracted into 300 µL of 50 mM sodium hydroxide/ methanol, 45/55% (v/v), within 15 s before being injected into the instrument. Enrichment factors ranged from 3.3 to 14.7 and limits of detection from 5.0 to 15.0 µg g-1. Coefficients of determination (R2) and %RSD were higher than 0.9962 and lower than 7.5%, respectively. The proposed method was efficiently applied for the extraction and quantitation of the three capsaicinoids in six cultivars of Capsicum annuum L. with percentage relative recoveries in the range of 92.0%-108.0%. DLLME was also scaled up for the isolation of the three major capsaicinoids providing purity greater than 98.0% as confirmed by liquid chromatography-mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) analysis, which significantly reduced the extraction time and organic solvent consumption.
RESUMO
Smartphone digital image colorimetry (SDIC), combined with solidification of floating organic drop-dispersive liquid-liquid microextraction (SFOD-DLLME), was proposed for the determination of iodate ions. A colorimetric box was designed to capture images of sample solutions. Factors affecting the efficiency of SDIC included type of phone, region of interest, position of camera, and distance between camera and sample solution. Optimum SFOD-DLLME conditions were achieved with 1-undecanol (500 µL) as the extraction solvent, ethanol (1.5 mL) as the disperser solvent within 20 s extraction time. Limit of detection (LOD) was found as 0.1 µM (0.2 µg g-1) and enrichment factors ranged between 17.4 and 25.0. Calibration graphs showed good linearity with coefficients of determination higher than 0.9954 and relative standard deviations lower than 5.6%. The proposed method was efficiently applied to determine iodate in table salt samples with percentage relative recoveries ranging between 89.3 and 109.3%.
Assuntos
Análise de Alimentos/métodos , Iodatos/análise , Microextração em Fase Líquida/métodos , Smartphone , Cloreto de Sódio na Dieta/análise , Calibragem , Colorimetria/instrumentação , Colorimetria/métodos , Análise de Alimentos/instrumentação , Processamento de Imagem Assistida por Computador , Limite de Detecção , Microextração em Fase Líquida/instrumentação , Solventes/químicaRESUMO
Switchable-hydrophilicity solvent liquid-liquid microextraction and dispersive liquid-liquid microextraction were compared for the extraction of piperine from Piper nigrum L. prior to its analysis by using high-performance liquid chromatography with UV detection. Under optimum conditions, limits of detection and quantitation were found as 0.2-0.6 and 0.7-2.0 µg/mg with the two methods, respectively. Calibration graphs showed good linearity with coefficients of determination (R2 ) higher than 0.9962 and percentage relative standard deviations lower than 6.8%. Both methods were efficiently used for the extraction of piperine from black and white pepper samples from different origins and percentage relative recoveries ranged between 90.0 and 106.0%. The results showed that switchable-hydrophilicity solvent liquid-liquid microextraction is a better alternative to dispersive liquid-liquid microextraction for the routine analysis of piperine in food samples. A novel scaled-up dispersive liquid-liquid microextraction method was also proposed for the isolation of piperine providing a yield of 102.9 ± 4.9% and purity higher than 98.0% as revealed by NMR spectroscopy.