Thais Matsue Uekane

Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g -1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

Studies on the volatile fraction composition of three native Amazonian-Brazilian fruits: Murici (Byrsonima crassifolia L., Malpighiaceae), bacuri (Platonia insignis M., Clusiaceae), and sapodilla (Manilkara sapota L., Sapotaceae)

The volatile fraction of murici, bacuri and sapodilla are here studied because of their increasing interest for consumers, abundance of production in Brazil, and the general demand for new flavors and aromas. Their volatile profiles were studied by two High Concentration Capacity Headspace techniques (HCC-HS), Headspace Solid Phase Microextraction (HS-SPME) and Headspace Sorptive Extraction (HSSE), in combination with GC-MS. Murici volatile fraction mainly contains esters (38%), carboxylic acids (19%), aldehydes (11%), alcohols (14%), others (13%) and sulfur compounds; bacuri is characterized by terpenes (41%), non-terpenic alcohols (24%), esters (15%), aldehydes (6%), and others (12%); sapodilla consists of esters (33%), alcohols (27%), terpenes (18%) and others (21%). The GC-MS component co-elution was overcome by GC×GC-qMS. The adoption of modern analysis technologies afforded to achieve a better knowledge of the volatile fraction composition of these fruit pulps by increasing substantially the number of compounds identified.

Evaluating Physicochemical and Rheological Characteristics and Microbial Community Dynamics during the Natural Fermentation of Cassava Starch

The traditional fermentation of cassava starch was investigated by a polyphasic approach combining (i) microbial community identification using conventional and molecular techniques, (ii) analyses of organic acids, volatile compounds, fermentation products and spin-lattice relation time and (iii) evaluation of technological properties, such as pasting properties, water absorption and water solubility indexes. Cassava fermentation microbiota was dominated by bacteria and yeasts genera. Bacteria genera include Lactobacillus, Leuconostoc, Lactococcus and Enterococcus. Lactobacillus was the prevalent genera responsible for the acidification of cassava fermentation by the production of organic acids and also aromatic compounds. Yeast community was dynamically adjusted through the cassava fermentation Pichia kudriavzevii and Issatchenkia orientalis were succeeded by Geotrichum candidum, Clavispora lusitaniae and Rhodotorula mucilaginosa. Candida rugosa, C. pararugosa, C. akabenensis, Cryptococcus albidus, Neurospora crassa and N. intermedia were found exclusively in sour cassava. The acidification of sour cassava was due to the production of acetic, lactic and succinic acids. Volatile compounds, including aliphatic and aromatic hydrocarbons, esters and terpenes contribute to the aroma and correspond to 23% of compounds found after fermentation and sun-drying treatment. The acidification and fermentation process reduced the peak viscosity, paste viscosity, breakdown viscosity and set back viscosity in cassava starch. Solid-state NMR relaxometry measures were associated to the expansion ability and indicated that the fermented and sun-dried products were more inclined to expansion. Loaf expansion ability and pasting temperatures were increased in sour cassava (fermented and sun-dried). The results showed here should be useful to standardize the manufacturing of cassava starch in Brazil, providing homogeneous and high quality products.

Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

A LC-ESI-MS/MS method was developed and validated according to the European Union decision 2002/657/EC, for the determination of tetracyclines (TCs) in chicken-muscle since Europe is one of the main markets for Brazilian products. Linearity of r > 0.9979, limits of quantification in the range of 7.0-35.0 ng/g, average recoveries of 89.38 - 106.27%, within-day and between-day precision were adequate for all TCs. The decision limit and the detection capability were 93.00-106.46 ng/g and 95.84-114.38 ng/g, respectively. This method is suitable for application in surveillance programmes of residues of TCs in chicken-muscle samples.

Comparison of High Performance Liquid Chromatography with Fluorescence Detector and with Tandem Mass Spectrometry methods for detection and quantification of Ochratoxin A in green and roasted coffee beans

Two analytical methods for the determination and confirmation of ochratoxin A (OTA) in green and roasted coffee samples were compared. Sample extraction and clean-up were based on liquid-liquid phase extraction and immunoaffinity column. The detection of OTA was carried out with the high performance liquid chromatography (HPLC) combined either with fluorescence detection (FLD), or positive electrospray ionization (ESI+) coupled with tandem mass spectrometry (MS-MS). The results obtained with the LC-ESI-MS/MS were specific and more sensitive, with the advantages in terms of unambiguous analyte identification, when compared with the HPLC-FLD.

Generation of Volatile Compounds from Carotenoids of Dunaliella bardawil Algae by Water Bath Heating and Microwave Irradiation

The volatile compounds formed by thermal degradation of the carotenoids present in Dunaliella bardawil were investigated by microwave irradiation (MW) and water bath heating (WB) in different conditions of temperature and time using central composite design. Volatiles extraction by solid phase microextraction (SPME) was optimized and performed at 40 °C for 15 minutes, and those in greater amount were quantified by a validated method of gas chromatography coupled to a quadrupole mass spectrometer (GC-qMS). Employing WB, 10, 12 and 120 ng mL-1 of β-cyclocitral, α-ionone e β-ionone, respectively, were obtained between 60 and 87 °C for 30-75 min, while by MW, 5, 5, 50 ng mL-1 were obtained between 75-107 °C for 1.5-2.8 min. Considering the shorter time of MW, it can be concluded that if the time necessary to obtain the best yield by WB is employed in multiple MW cycles, an amount 10 times greater of those compounds would be obtained by MW than by WB. The results suggest a new biotechnology application for the carotenoids of the microalgae of the Dunaliella genus.