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Application of quality-by-design approach in the analytical method development for quantification of sugars in sugarcane honey by reversed-phase liquid chromatography
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Advisor(s)
Abstract(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.
Description
Keywords
Sugarcane honey Sugar Typicality Quality-by-design USA-LLE LC-RI . Faculdade de Ciências Exatas e da Engenharia Centro de Química da Madeira
Citation
Silva, P., Silva, C. L., Perestrelo, R., Nunes, F. M., & Câmara, J. S. (2020). Application of quality-by-design approach in the analytical method development for quantification of sugars in sugarcane honey by reversed-phase liquid chromatography. Food Analytical Methods, 13, 1634-1649. https://doi.org/10.1007/s12161-020-01767-7
Publisher
Springer