Determination of butylated hydroxytoluene in food samples by high-performance liquid chromatography with ultraviolet detection and gas chromatography/mass spectrometry

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and compared with a gas chromatography/mass spectrometry (GC/MS) method for determining butylated hydroxytoluene (BHT) in foodstuffs as a result of migration from plastic packaging. Similar extraction procedures were used in both methods. BHT was quantitated using an external standard in the HPLC method and an internal standard in the GC/MS method. Both methods presented good linearity (r(2) > or = 0.9917) and low detection limits. Recoveries obtained with the HPLC method (chicken meat, 95.8%, and Gouda cheese, 83.9%) were better than with the GC/MS method (chicken meat, 85.6%, and Gouda cheese, 71.3%).     

Analytical method for the simultaneous determination of polyfunctional amines used as monomers in the manufacture of food packaging materials

This paper describes the development of a multi-analyte method for the determination of polyfunctional amines commonly used as monomers in the manufacture of food contact materials. Amines were analyzed by high-performance-liquid chromatography with diode-array detection (HPLC-DAD) after derivatization with dansyl chloride. The chromatographic analysis and the derivatization conditions were optimized. The proposed method was validated in terms of linearity, limits of detection and repeatabilities. The method showed an excellent sensitivity (LOD≤0.05 μg/mL) and appropriate repeatabilites (RSD (n=7)≤5%)). LC-MS/MS was used as a confirmatory technique. The stability of the amines in five food simulants (distilled water, 3% acetic acid, 10% ethanol, 50% ethanol and olive oil) under the most common testing conditions (10 days at 40 °C) was also studied. Results showed that amines had an acceptable stability in aqueous simulants but in the olive oil a loss of 100% was observed for all analytes.     

Ultra-high pressure LC determination of glucosamine in shrimp by-products and migration tests of chitosan films

Chitosan, a multiple applications molecule, was isolated from shrimp by-products by fermentation. The amount of chitosan in the solid fraction of the fermented extract was measured after its conversion in the respective glucosamine units. The procedure includes an acid hydrolysis (110 °C, 4 h with HCl 8 M) and a derivatization with 9-fluorenylmethyl chloroformate (Fmoc-Cl). Ultra-high-pressure liquid chromatography method was developed and optimized. Excellent peaks resolution was achieved in just 10 min. The method was evaluated in what concerns to validation parameters such as linearity, repeatability, quantification limit, and recovery. Migration tests of films prepared with chitosan were carried out in two simulants: ultrapure water and ethanol 95% (v/v).     

Computational models of music perception and cognition I: The perceptual and cognitive processing chain

We present a review on perception and cognition models designed for or applicable to music. An emphasis is put on computational implementations. We include findings from different disciplines: neuroscience, psychology, cognitive science, artificial intelligence, and musicology. The article summarizes the methodology that these disciplines use to approach the phenomena of music understanding, the localization of musical processes in the brain, and the flow of cognitive operations involved in turning physical signals into musical symbols, going from the transducers to the memory systems of the brain. We discuss formal models developed to emulate, explain and predict phenomena involved in early auditory processing, pitch processing, grouping, source separation, and music structure computation. We cover generic computational architectures of attention, memory, and expectation that can be instantiated and tuned to deal with specific musical phenomena. Criteria for the evaluation of such models are presented and discussed. Thereby, we lay out the general framework that provides the basis for the discussion of domain-specific music models in Part II.     

Determination of diphenylbutadiene by liquid chromatography-UV-fluorescence in foodstuffs

Diphenylbutadiene (DPBD) is an optical brightener incorporated into a wide range of polymeric materials. Framed in the FOODMIGROSURE project, it was chosen as a model migrant to study the migration kinetics from polymeric materials in relevant foodstuffs. An analytical method was developed and optimized for the DPBD determination in foods. The sample preparation procedure uses both hexane and acetonitrile as extraction solvents, followed by high-performance liquid chromatography (HPLC) analysis. HPLC analysis was performed using UV detection at a wavelength of 330 nm, and fluorescence detection achieved with excitation and emission wavelengths of 330 and 375 nm, respectively. Good linearity and recovery were achieved. Data are reported.     

Determination ofm-xylylenediamine in the official EU food simulant olive oil

Summary EU Directive 90/128/EEC prescribes a specific migration limit (SML) of 0.05 mg kg⁻¹ for the aliphatic diaminem-xylylenediamine (XDA) into food or food simulants, but there is no generally accepted method of analysis available for testing compliance with this restriction.m-XDA has been determined in olive oil (EU food simulant for fatty foods) by high-performance liquid chromatography (HPLC) with fluorescence detection, after extraction into an aqueous phase and derivatization with fluorescamine. The method is appropriate for the quantitative determination ofm-XDA at a minimum level of 0.02 mg kg⁻¹ in this food simulant. The method should also be applicable to other fatty-food simulants (sunflower oil and HB 307).     

Determination of vitamin E and carotenoid pigments by high performance liquid chromatography in shell of Chionoecetes opilio

This study reports the optimization of a method for the determination of vitamin E and carotenoids in shells of Chionoecetes opilio samples by online HPLC coupled with UV-vis and fluorescence detectors. The carotenoids were determined with diode-array detector (lambda 450 nm) and vitamin E with fluorescence detection (lambda(ex) 288, lambda(em) 331 nm). Two extractions methods were compared, saponification followed by an extraction step and a simple extraction with acetone. The last one was selected because allows to determine all compounds. Linearity, precisions and recoveries achieved for all compounds were satisfactory. Mean concentrations (mg per 100 g dry weight) were; 23.3 for vitamin E, 9.49 for astaxanthin and 0.2 mg for beta-carotene.     

Determination of hexanal as indicator of the lipidic oxidation state in potato crisps using gas chromatography and high-performance liquid chromatography

Hexanal (an oxidative state indicator) formed in the headspace of potato crisps during storage was evaluated using two different procedures. First, solid-phase microextraction, an innovative sampling preparation methodology was used. It consisted on the absorption of analytes directly from samples and subsequent thermal desorption on the gas chromatograph (GC) injector. Then, a reversed-phase high-performance liquid chromatographic technique (HPLC) was employed to quantify hexanal in the form of 2,4-dinitrophenylhydrazone derivative. Methods were evaluated in what concerns to validation parameters such as linearity, repeatibility and detection limit. GC (LOD = 1 ng/ml) method resulted in more sensitive method than HPLC (LOD = 9 ng/ml). The most suitable technique for hexanal measurement was selected.     

Determination of the alcohol denaturants denatonium benzoate (bitrex) and diethyl phthalate by direct flow injection APCI-MS analysis

The recently developed tandem technique, mass spectroscopy with atmospheric-pressure chemical ionization (APCI-MS) coupled with direct flow injection, was applied to the determination of Bitrex (denatonium benzoate) and diethyl phthalate in ethanol. The compounds were indentified from their total-ion chromatograms(m/z 50-500) and, simultancously, quantified using selected-ion chromatograms recorded at m/z 223 for diethyl phthalate and m/z 325 for Bitrex. Operating conditions were optimized for soft ionization (positive ion-mode) with fragmentation limited to that necessary for analyte identification, which was by the external-standard method. Calibration curves were rectilinear in the concentration rages 2-30 μg ml^?1 (Bitrex) and 0.075-1.2% v/v (diethyl phthalate); measurement precision (RSDs were 11.48% for Bitrex and 2.22% for diethyl phthalate), and detection limits (0.017 μg ml^?1 and 0.010% v/v, respectively) were adequate for simiultaneous quantitation and with high sensitivity. The lack of any sample pretreatment and the use of flow-injection analysis meant that the procedure was moere straightforward and rapid than previously reported methods.