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1.
Ultrason Sonochem ; 21(6): 2131-7, 2014 Nov.
Article in English | MEDLINE | ID: mdl-24751292

ABSTRACT

The effects of ultrasound application on skim milk (10% w/w total solids at natural pH 6.7 or alkali-adjusted to pH 8.0) prior to the renneting of milk at pH 6.7 were examined. Skim milk, made by reconstituting skim milk powder, was sonicated at 20kHz and 30°C (dissipated power density 286kJkg(-1)) in an ultrasonic reactor. The rennet gelation time, curd firming rate, curd firmness, and the connectivity of the rennet gel network were improved significantly in rennet gels made from milk ultrasonicated at pH 8.0 and re-adjusted back to pH 6.7 compared to those made from milk sonicated at pH 6.7. These renneting properties were also improved in milk sonicated at pH 6.7 compared to those of the non-sonicated control milk. The improvements in renneting behavior were related to ultrasound-induced changes to the proteins in the milk. This study showed that ultrasonication has potential to be used as an intervention to manipulate the renneting properties of milk for more efficient manufacturing of cheese.


Subject(s)
Chymosin/metabolism , Milk/metabolism , Sonication , Animals , Blood Proteins/metabolism , Chromatography, Gel , Hydrogen-Ion Concentration , Milk/chemistry , Particle Size
2.
J Dairy Res ; 81(2): 146-55, 2014 May.
Article in English | MEDLINE | ID: mdl-24351847

ABSTRACT

Reconstituted skim milks (10 % w/w total solids, pH 6·7-8·0) were ultrasonicated (20, 400 or 1600 kHz at a specific energy input of 286 kJ/kg) at a bulk milk temperature of <30 °C. Application of ultrasound to milk at different pH altered the assembly of the casein micelle in milk, with greater effects at higher pH and lower frequency. Low frequency ultrasound caused greater disruption of casein micelles causing release of protein from the micellar to the serum phase than high frequency. The released protein re-associated to form aggregates of smaller size but with surface charge similar to the casein micelles in the original milk. Ultrasound may be used as a physical intervention to alter the size of the micelles and the partitioning of caseins between the micellar and serum phases in milk. The altered protein equilibria induced by ultrasound treatment may have potential for the development of milk with novel functionality.


Subject(s)
Caseins/chemistry , Food Handling/methods , Micelles , Milk/chemistry , Sonication , Animals , Food, Preserved , Hydrogen-Ion Concentration , Particle Size , Protein Aggregates , Solubility , Sound
3.
Anal Chim Acta ; 781: 33-40, 2013 Jun 05.
Article in English | MEDLINE | ID: mdl-23684462

ABSTRACT

Blood plasma collected from adult fish (black bream, Sparidae) exposed to a dose of 5 mg kg(-1) 17ß-estradiol underwent metabonomic profiling using nuclear magnetic resonance (NMR). An extension of the orthogonal 2 projection to latent structure (O2PLS) analysis, tO2PLS, was proposed and utilized to classify changes between the control and experimental metabolic profiles. As a bidirectional modeling tool, O2PLS examines the (variable) commonality between two different data blocks, and extracts the joint correlations as well as the unique variations present within each data block. tO2PLS is a proposed matrix transposition of O2PLS to allow for commonality between experiments (spectral profiles) to be observed, rather than between sample variables. tO2PLS analysis highlighted two potential biomarkers, trimethylamine-N-oxide (TMAO) and choline, that distinguish between control and 17ß-estradiol exposed fish. This study presents an alternative way of examining spectroscopic (metabolite) data, providing a method for the visual assessment of similarities and differences between control and experimental spectral features in large data sets.


Subject(s)
Magnetic Resonance Spectroscopy/methods , Metabolomics/methods , Perciformes/metabolism , Software , Animals , Biomarkers/analysis , Biomarkers/metabolism , Choline/analysis , Choline/metabolism , Estradiol/pharmacology , Metabolome , Methylamines/analysis , Methylamines/metabolism , Models, Biological
4.
Anal Biochem ; 429(1): 1-7, 2012 Oct 01.
Article in English | MEDLINE | ID: mdl-22750518

ABSTRACT

Generalized two-dimensional (Gen2D) correlation analysis and hybrid correlation analysis have been applied to a series of dynamic (31)P nuclear magnetic resonance (NMR) spectra to monitor the in vivo metabolic changes of the plant pathogen Phytophthora palmivora in the presence and absence of phosphonate over an 18-h period. Results indicate that phosphonate exposure causes cleavage in organism polyphosphate chains as well as an increase in total sugar phosphates. In the presence of phosphonate, the NMR resonances attributed to terminal polyphosphate phosphorus reduced at a lower rate than those of middle polyphosphate phosphorus, indicating a change in average chain length and suggesting cleavage in the middle of the chain as well as at the ends. The correlation analysis techniques serve to identify and confirm spectral regions undergoing major change in the time-series data and facilitate the analysis of these dynamic changes.


Subject(s)
Magnetic Resonance Spectroscopy/methods , Phosphorus/analysis , Phytophthora/chemistry , Multivariate Analysis , Phosphorus/chemistry
5.
Anal Chem ; 82(11): 4501-9, 2010 Jun 01.
Article in English | MEDLINE | ID: mdl-20441219

ABSTRACT

The present study describes a preparative gas chromatographic (GC) approach employed to study a series of products arising from reaction of phenylacetylene with para-substituted aryl-iodides under Sonogashira catalysis conditions. GC analysis resolves the isomers from each reaction; however, it cannot provide structural details (their MS data are virtually identical). Since classical liquid chromatography cannot resolve the isomers, preparative-scale GC is the only practical approach to provide further spectroscopic characterization of the isomers. The products are well separated by GC so a single thick-film capillary column is adequate for this case, with operation up to approximately +300 degrees C. By collection of 50+ repeat injections, sufficient material could be isolated for (1)H NMR spectral analysis of the isomers, and for one isomer (isomer I) of a number of analogous related catalytic reaction mixtures, X-ray crystal structure determination enabled complete structural elucidation (absolute configuration) of the substitution pattern of the structure of this isomer. This confirmed isomer I to be the 2-para-aryl-substituted 1,3,5-triphenylbenzene product in all cases. (1)H NMR spectra of isomer I products generally had similar patterns but differed markedly from the second major isomer product (isomer II).


Subject(s)
Benzene/chemistry , Crystallography, X-Ray/methods , Gas Chromatography-Mass Spectrometry/methods , Magnetic Resonance Spectroscopy/methods , Acetylene/analogs & derivatives , Acetylene/chemistry , Catalysis , Iodine/chemistry , Isomerism
6.
Anal Chim Acta ; 652(1-2): 173-9, 2009 Oct 12.
Article in English | MEDLINE | ID: mdl-19786178

ABSTRACT

Spectroscopic studies of complex clinical fluids have led to the application of a more holistic approach to their chemical analysis becoming more popular and widely employed. The efficient and effective interpretation of multidimensional spectroscopic data relies on many chemometric techniques and one such group of tools is represented by so-called correlation analysis methods. Typical of these techniques are two-dimensional correlation analysis and statistical total correlation spectroscopy (STOCSY). Whilst the former has largely been applied to optical spectroscopic analysis, STOCSY was developed and has been applied almost exclusively to NMR metabonomic studies. Using a (1)H NMR study of human blood plasma, from subjects recovering from exhaustive exercise trials, the basic concepts and applications of these techniques are examined. Typical information from their application to NMR-based metabonomics is presented and their value in aiding interpretation of NMR data obtained from biological systems is illustrated. Major energy metabolites are identified in the NMR spectra and the dynamics of their appearance and removal from plasma during exercise recovery are illustrated and discussed. The complementary nature of two-dimensional correlation analysis and statistical total correlation spectroscopy are highlighted.


Subject(s)
Exercise , Metabolomics/methods , Nuclear Magnetic Resonance, Biomolecular/methods , Blood Chemical Analysis , Electronic Data Processing , Humans
7.
Anal Chim Acta ; 629(1-2): 128-35, 2008 Nov 23.
Article in English | MEDLINE | ID: mdl-18940329

ABSTRACT

A wine fermentation has been monitored on a daily basis by (1)H NMR spectroscopy. Following data pre-processing that includes synthesis of the spectra to ensure all peaks are of constant half-width, the series of spectra were examined using generalised two-dimensional correlation techniques. Synchronous and asynchronous data maps have been generated and employed to interpret the changes in the fermentation process as a function of time. The results illustrate the potential of high resolution NMR with multivariate data analysis as a tool for process monitoring and the manner in which two-dimensional correlation mapping can aid in data interpretation.

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