RESUMO
Mid-infrared analysis of reconstituted milk is proposed as a feasible solution for the detection of milk powder adulteration regardless of the blending practice. To challenge the concept, skim milk powders were spiked with three of the most reactive/unstable of potential milk adulterants: semicarbazide hydrochloride, ammonium sulfate and cornstarch. To create the wet-blended set, a fraction of each sample was reconstituted and re-spray dried at laboratory scale with a benchtop spray dryer. Dry and wet-blended adulterated samples were reconstituted prior to mid-infrared measurement and projected onto a one-class classifier SIMCA model for reconstituted skim milk. Quantitative sensitivities, determined from the normalized orthogonal distances, were compared. Although the non-industrial spray drying introduced a spectroscopic bias, as revealed by the control samples, the non-targeted mid-infrared model showed comparable sensitivities for both blending practices once the main bias-rich spectral regions were removed, validating thereby the proposed concept.
Assuntos
Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Leite/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Sulfato de Amônio/química , Animais , Análise de Alimentos/economia , Modelos Teóricos , Pós/química , Semicarbazidas/química , Amido/químicaRESUMO
INTRODUCTION: Western flower thrips (Frankliniella occidentalis) are among the most serious crop pests worldwide. Control of thrips mainly depends on pesticides, excessive use of which leads to human health risks and environmental contamination. As an alternative, we study host plant resistance to thrips. OBJECTIVE: To apply nuclear magnetic resonance spectroscopy (NMR) metabolomics to study host plant resistance to thrips in wild and cultivated tomatoes. METHODOLOGY: Ten wild species and 10 cultivated tomato lines were compared. Five replicates of each species and lines were used for a thrips bioassay while another five replicates were used for the metabolomic analysis. The three most resistant and susceptible wild species, and cultivated lines, as identified by the thrips bioassay, were used for the metabolomics, performed by (1)H NMR spectroscopy followed by principal component analysis. RESULTS: Wild and cultivated tomatoes differed significantly in thrips resistance. Only wild tomatoes were thrips-resistant, among which Lycopersicon pennellii and L. hirsutum exhibited the lowest thrips damage. Their (1)H NMR-based metabolomic profiles were significantly different from those of thrips-susceptible tomatoes. Thrips-resistant tomatoes contained acylsugars, which are known for their negative effect on herbivores. CONCLUSION: The identification of acylsugars as a resistance factor for thrips in tomato proves that NMR-based metabolomics an important tool to study plant defences, providing fundamental information for the development and realisation of herbivore resistance breeding programmes in agricultural crops.
Assuntos
Afídeos/patogenicidade , Metabolômica , Solanum lycopersicum/metabolismo , Animais , Bioensaio , Solanum lycopersicum/parasitologia , Ressonância Magnética Nuclear BiomolecularRESUMO
In addition to sample solubility constraints, the use of polarity gradients in normal-phase centrifugal partition chromatography (CPC) for the purification of complex mixtures is also limited by the instability of biphasic systems as a consequence of dramatic changes in the settling times along the gradient, leading in many cases to column bleeding when working under maximum efficiency conditions. In this paper an electrostriction approach is proposed as a strategy in reversed-phase CPC to fractionate intermediate polarity extracts in a single run by bringing its components into the "sweet spot" in a controlled fashion through a stepwise reduction of salt concentration in the aqueous mobile phase. The salting-out gradient method was successfully tested with the separation of the major chlorogenic acids (CGAs, hydroxycinnamoylquinic acids) present in green coffee beans (5-caffeoylquinic acid (5-CQA), 5-feruloylquinic acid (5-FQA) and 3,5-dicaffeoylquinic acid (3,5-diCQA)) using ethyl acetate-hexane as the stationary phase and an ionic gradient of LiCl (5.0, 2.5 and 0.1M) as the mobile phase in one case and (NH(4))(2)SO(4)/KNO(3) (3.0 and 1.5M/1.5M) in another. Regioisomers of each chlorogenic acid obtained by base-catalyzed isomerisation were also separated by CPC using isocratic elution. The best resolution for both FQAs and diCQAs was achieved with a chloroform-n-butanol-0.01M pH 2.5 phosphate buffer (84:16:100; v/v) system, while CQAs were best isolated using chloroform-n-butanol-0.01M pH 2.5 phosphate buffer/5.0M LiCl (82:18:100; v/v).
Assuntos
Centrifugação/métodos , Ácido Clorogênico/isolamento & purificação , Coffea/química , Distribuição Contracorrente/métodos , Ácido Quínico/análogos & derivados , Sementes/química , Ácido Clorogênico/química , Cloreto de Lítio/química , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Ácido Quínico/química , Ácido Quínico/isolamento & purificação , Sais/química , Solventes/químicaRESUMO
Three labdane diterpenes 15,16-epoxy-6-hydroxylabda-5,8,13(16),14-tretraen-7-one (leojaponin), (9alpha,13S);15,16-diepoxy-7beta-hydroxylabd-14-en-6-one (13-epi-preleoheterin), and (9alpha,13R);15,16-diepoxy-6beta-hydroxylabd-14-en-7-one (iso-preleoheterin) were isolated from the leaves of Leonurus japonicus, in addition to the previously reported preleoheterin. The structure elucidations were made based on analysis of their spectroscopic data.