RESUMEN
The characterization of amaranth seeds (Amaranthus spp.) was developed for Amaranthus hypochondriacus, Amaranthus cruentus, and Amaranthus dubius. The elemental concentrations were determined by inductively coupled plasma optic atomic spectroscopy. Pattern recognition methods were used for the characterization of seed samples: nonsupervised methods included principal components analysis and cluster analysis; supervised methods were linear discriminant analysis and partial least squares discriminant analysis (PLS-DA). Informed are the concentrations of the following elements: Ag, Al, Ba, Ca, Co, Cr, Cu, Fe, K, La, Li, Mg, Mn, Mo, Na, Ni, P, S, Sr, V, Zn, and Zr. The lowest mineral content was found in A. hypochondriacus, and the highest one was found in A. dubius. For the classification, selected variables for all multivariate methods were Ba, Cr, Li, Mn, Ni, S, and Sr. Nonsupervised methods allowed us to distinguish between the three species of amaranth; however, PLS-DA supervised methods showed the best prediction ability.
Asunto(s)
Amaranthus , Metales/análisis , Semillas/química , Semillas/clasificación , Análisis Discriminante , Análisis de los Mínimos Cuadrados , Minerales/análisis , Reproducibilidad de los ResultadosRESUMEN
A new method for the simultaneous determination of amoxicillin trihydrate (AMT) and sodium diclofenac (DIC) in pharmaceutical formulations is proposed. The resolution of binary mixtures of these drugs has been accomplished by using partial least squares (PLS) regression analysis. The model was obtained from UV spectral data and validated by internal cross-validation; it was used to find the concentration of analytes in some commercial samples. The method was applied in the concentration ranges of 0-120.0 mg L(-1) for AMT and 0-16.0 mg L(-1) for DIC, allowing a rapid, accurate and precise simultaneous estimation of the concentration of both analytes of interest in the presence of small amounts of different, unmodelled, absorbing excipients, in spite of their important spectral overlapping. The accuracy, precision and figures of merit (FOM) for AMT and DIC were calculated. This new method proved to be useful for a fast and simultaneous determination of AMT and DIC in pharmaceutical formulations.
Asunto(s)
Amoxicilina/análisis , Diclofenaco/análisis , Preparaciones Farmacéuticas/química , Análisis de los Mínimos Cuadrados , Espectrofotometría UltravioletaRESUMEN
INTRODUCTION: The chemometric characterisation of two plants frequently used as food and medicinal species, Achyrocline satureioides and Achyrocline venosa (Asteraceae: Gnaphalieae), was carried out based on their mineral composition. Both species, known by the common name of 'marcelas', are very similar in their morphological features but they have different medicinal and food properties. OBJECTIVE: To develop multivariate models for the classification of A. satureiodes and A. venosa based on their mineral content. METHODOLOGY: The analytic determinations were made by means of inductively coupled plasma optical emission spectrometry from aerial parts of the plants. An internal standard was used to evaluate the accuracy in the sample treatment and the recovery of toxic elements was studied. The multivariate methods used include principal components analysis, cluster analysis and linear discriminant analysis. RESULTS: Classification for both A. satureioides and A. venosa was successful in all cases using only four variables: aluminium, iron, magnesium and sulphur content. The concentrations of the following elements were determined: Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, La, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sr, Ti, V, Y and Zn. CONCLUSIONS: This method is useful to identify both species in raw material in order to detect eventual errors of selection.
Asunto(s)
Achyrocline/química , Minerales/análisis , Plantas Comestibles/química , Plantas Medicinales/química , Análisis por Conglomerados , Análisis Discriminante , Indicadores y Reactivos , Análisis de Componente Principal , Programas Informáticos , América del Sur , OligoelementosRESUMEN
A method for the determination of oleic acid in sunflower seeds is proposed. One hundred samples of sunflower seeds were analyzed by near-infrared diffuse reflectance spectroscopy (NIRDRS). The direct measures were realized in ground and sifted seeds. The PLS multivariate calibration model was obtained using first derivate absorbance values as response matrix, while the oleic acid concentration matrix was obtained analyzing the seed samples by gas chromatography with a flame ionization detector (GC-FID). The NIRDRS-PLS model was validated externally using unknown samples of sunflower seeds. The accuracy and precision of the method was evaluated using GC as reference method. The following figures of merit (FOM) were obtained: LOD=3.4% (w/w); LOQ=11.3% (w/w); SEN=8x10(-5); SEL=0.15; analytical sensibility (gamma)=1.5 and linear range (LR)=18.1-89.2% (w/w). This method is useful for the fast determination of oleic acid in sunflower seeds and for quality control of raw materials.
Asunto(s)
Helianthus/química , Ácido Oléico/análisis , Semillas/química , Espectroscopía Infrarroja Corta/métodos , Algoritmos , Calibración , Cromatografía de Gases , Análisis Multivariante , Ácido Oléico/química , Ácido Oléico/normas , Control de Calidad , Reproducibilidad de los ResultadosRESUMEN
A new method to determine a mixture for sweetener sodium saccharin and aspartame in commercial noncaloric sweeteners is proposed. A classical full factorial design for standards was used in the calibration step to build the partial least-squares (PLS-2) model. Instrumental data were obtained by means of UV-visible spectrophotometry. Salicylic acid was used as an internal standard to evaluate the adjustment of the real samples to the PLS model. The concentration of analytes in the commercial samples was evaluated using the obtained model by UV spectral data. The PLS-2 method was validated by capillary zone electrophoresis (CZE), finding in all cases a relative error of less than 11% between the PLS-2 and the CZE methods. The proposed procedure was applied successfully to the determination of saccharin and aspartame in noncaloric commercial sweeteners.