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- Effect of processing and storage on the volatile profile of sugarcane honey: A four-year studyPublication . Silva, Pedro; Freitas, Jorge; Nunes, Fernando M.; Câmara, José S.Sugarcane honey (SCH) is a syrup from Madeira Island recognized by its unique and excellent aroma, associated to volatile organic compounds (VOCs) generated during the well-defined five stages of its traditional making process. The establishment of volatile profile throughout all SCH-making stages during four years, allowed the evaluation of the influence of each stage in the typical characterisitcs of SCH. One hundred eighthy seven VOCs were identified, being associated to several origins and formation pathways. VOCs formed during stage 1 and 2 were originate from raw material, and its oxidation (i.e. enzymatic browning) and thermal degradation (i.e. lipid oxidation, Maillard reactions, Strecker degradation). In stage 3 and 4, the caramelization and melanoidin degradation also occurred, while in stage 5, the thermal degradation continues, followed by microbial activity. Chemometric analysis allowed to identify 35 VOCs as potential markers for processing control by the producers and as guarantee of the typicality and authenticity of SCH. Based on the obtained results, we propose for the first time an innovative schematic diagram explaining the potential reactions and pathways for VOCs formation during the different steps of the SCH production.
- Application of quality-by-design approach in the analytical method development for quantification of sugars in sugarcane honey by reversed-phase liquid chromatographyPublication . Silva, Pedro; Silva, Catarina L.; Perestrelo, Rosa; Nunes, Fernando M.; Câmara, José S.Produced in Madeira Island from regional sugarcane cultivars through a traditional manufacturing and storage process, sugarcane honey (SCH) is a black syrup recognized by its excellent quality. Its economic value has led to the emergence of adulterated SCH, whereby the identification of molecular markers became an essential task in order to overcome the fraudulent activities, protect its authenticity, and guarantee the consumer safety. In the present study, an analytical strategy based on ultrasound-assisted liquid liquid extraction (USA-LLE) followed by reversed-phase liquid chromatography with a refractive index detector (LC-RI) was developed for the determination of sugars (glucose, fructose, sucrose, xylose, and mannose) in SCH samples from certified producers, supported on analytical quality-by-design (AQbD) approach, as a useful tool to establish its typicality. The application of AQbD was based on analytical risk assessment, multivariate statistics and quality control procedures for definition of the Method Operable Design Region (MODR). The optimal conditions into MODR were accomplished using BEH Amide column operating at a temperature of 80 °C and a flow rate of 300 μL min−1 , with a mobile phase composed by acetone and water (85:15, v v−1 ) at a flow rate of 1.0 mL min−1 . The robustness was determined by Monte Carlo simulation and capability analysis. The concentration-response function for all sugars was described by polynomial models. Accuracy was presented by recovery values between 98.2 and 119.5%. The analytical figures of merit validated the utility of AQbD in the systematic design of a LC-RI method with fine sensitivity for sugar analysis in SCH.