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Slice shear force (SSF) and laser diffraction, considered faster methodologies, for measuring beef instrumental tenderness and sarcomere length, were compared with reference methodologies Warner-Bratzler shear force (WBSF) and phase contrast microscopy. Striploin samples (n = 74) were analyzed for pH, sarcomere length, instrumental tenderness, myofibrillar fragmentation index, and sensorial tenderness. Pearson's correlation measured the association of meat evaluation methods with residual analysis of the multivariate analysis of variance model. The n-dimensional profile to evaluated methods was presented by biplot to identify the behavior of the correlation between the methods (variables). There was moderate correlation between SSF and WBSF (r = .63; p < .01) and both presented moderate correlation with sensorial tenderness (r = - .62 and -.55, to SSF and WBSF, respectively; p < .01). However, WBSF was more efficient to classify samples as tender (68%) than SSF (47%), comparing with sensorial tenderness (80%). There was a moderate correlation for laser and microscopy for sarcomere length (r = .57; p < .01). Sarcomeres were shorter when measured by laser than microscopy. Either with low correlation coefficients, sarcomere measured by laser (r = .29; p < .05) presented higher correlation with sensorial tenderness than with microscopy (r = .22; p < .10). Results highlighted that SSF was faster and easier to run, while WBSF was more appropriate to classify samples by sensorial tenderness grades. Laser diffraction is more suitable to explain effects on tenderness; however, microscopy revealed results of sarcomere length that were more realistic, once laser can underestimate sarcomeres.

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Different types of hair were submitted to different milling procedures and their resulting powders were analyzed by scanning electron microscopy (SEM) and laser diffraction (LD). SEM results were qualitative whereas LD results were quantitative and accurately characterized the hair powders through their particle size distribution (PSD). Different types of hair were submitted to an optimized milling conditions and their PSD was quite similar. A good correlation was obtained between PSD results and ketamine concentration in a hair sample analyzed by LC-MS/MS. Hair samples were frozen in liquid nitrogen for 5min and pulverized at 25Hz for 10min, resulting in 61% of particles <104µm and 39% from 104 to 1000µm. Doing so, a 359% increment on ketamine concentration was obtained for an authentic sample extracted after pulverization comparing with the same sample cut in 1mm fragments. When milling time was extended to 25min, >90% of particles were <60µm and an additional increment of 52.4% in ketamine content was obtained. PSD is a key feature on analysis of pulverized hair as it can affect the method recovery and reproducibility. In addition, PSD is an important issue on sample retesting and quality control procedures.

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ABSTRACT The physicochemical attributes of emulsified systems are influenced by the characteristics of their internal phase droplets (concentration, size and morphology), which can be modified not only by the formulation components, but also by the analytical methodology employed. Thus, the aim of this work involved the physicochemical characterization of cosmetic emulsions obtained from different surfactants, as well as the introduction of the optical coherence tomography (OCT) as the analytical technique employed for the morphological characterization and particle size determination of the formulations. Three emulsions were prepared, differing at the type and concentration of the surfactant used, and their droplet sizes were evaluated through optical microscopy, laser diffraction and OCT. The microscopic analysis and the laser diffraction techniques provided an average particle size minor than 6.0 µm, not detected by the OCT technique, which could identify only bigger particles of the emulsified systems' internal phase. The results testify that OCT was suitable for the morphological characterization of cosmetic emulsions; however, the technique needs to be improved to ensure a better sensitivity in the analysis of smaller particles.

RESUMO Os atributos físico-químicos de sistemas emulsionados são influenciados pelas características de suas gotículas de fase interna (concentração, tamanho e morfologia), as quais podem ser modificadas não apenas pelos componentes da formulação, mas também pela metodologia analítica empregada. Desta forma, o objetivo deste trabalho envolveu a caracterização físico-química de emulsões cosméticas obtidas a partir de diferentes tensoativos, bem como a introdução da tomografia de coerência óptica (OCT) como a técnica analítica utilizada para a caracterização morfológica e determinação do tamanho de partícula das formulações. Três emulsões foram preparadas, diferindo no tipo e concentração do tensoativo empregado, e seus tamanhos de gotícula foram avaliados por meio das técnicas de microscopia óptica, difração a laser e OCT. As técnicas de microscopia óptica e difração a laser forneceram tamanhos de partícula médios menores de 6.0 µm, não detectados pela técnica de OCT, que permitiu apenas a identificação de partículas maiores pertencentes à fase interna dos sistemas emulsionados. Os resultados reforçam a introdução da OCT como metodologia promissora para a caracterização morfológica de emulsões cosméticas; no entanto, a técnica requer aprimoramento para garantir maior sensibilidade na análise de partículas de menor tamanho.

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