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- Fingerprint targeted compounds in authenticity of sugarcane honey: an approach based on chromatographic and statistical dataPublication . Silva, Pedro; Silva, Catarina L.; Perestrelo, Rosa; Nunes, Fernando M.; Câmara, José S.ugarcane honey (SCH) is a black syrup recognized by its excellent quality, being produced in Madeira Island using the regional sugarcane cultivars and following a traditional and peculiar manufacturing and storage processes. However, some low-quality commercial products have been labeled as SCH but do not respect its criteria, revealing the need of develop powerful strategies in order to detect and prevent adulterations. The knowledge of furanic derivatives (FDs) profile, produced during browning reactions that occurs during food processing and storage, emerged as a promising strategy in food quality and fraud prevention. Therefore, the aim of this study was to establish the FDs profiling of typical SCH produced by certified and non-certified producers, in different geographical regions (Madeira and Brazil), based on microextraction by packed sorbent (MEPS) combined with ultra-high performance liquid chromatography (UHPLC) as a useful approach to define its typicality and authenticity. These parameters are defined through the differentiation and discrimination of FDs profiles among other sugarcane-derived products using multivariate statistical analysis (ANOVA with post-hoc Tukey, principal components analysis, partial least square, linear discriminant analysis and hierarchical clustering). The results demonstrated that SCH samples from non-certified producers present the highest levels of FDs. In addition, SCH samples from Brazil present higher levels of FDs than samples from Madeira region. The obtained results revealed that the proposed approach is a valuable strategy to establish the typicality of SCH, ensuring its quality, authenticity, safety control and a useful support regarding the application of SCH from Madeira Island to EU certification.
- A useful strategy based on chromatographic data combined with quality-by-design approach for food analysis applications. The case study of furanic derivatives in sugarcane honeyPublication . Silva, Pedro; Silva, Catarina L.; Perestrelo, Rosa; Nunes, Fernando M.; Câmara, José S.Sugarcane honey (SCH) is one of the Madeira Island products par excellence and it is now popular worldwide. Its sui generis and peculiar sensory properties, explained by a variety of volatile compounds including furanic derivatives (FDs), arise mainly from manufacturing and storage conditions. A simple high-throughput approach based on semi-automatic microextraction by packed sorbent (MEPS) combined with ultra-high performance liquid chromatography (UHPLC) was developed and validated for identification and quantification of target FDs in sugarcane honey. A Quality-by-Design (QbD) approach was used as a powerful strategy to optimize analytical conditions for high throughput analysis of FDs in complex sugar-rich food matrices. The optimum point into MEPS-Method Operable Design: Region (MODR) was obtained with R-CX sorbent, acetonitrile (ACN) as elution solvent, three loading cycles and 500μL of sample volume. The optimum point into UHPLC-MODR was obtained with a CORTECS column operating at a temperature of 50°C, ACN as eluent and a flow rate of 125μLmin-1. The robustness was demonstrated by Monte Carlo simulation and capability analysis for estimation of residual errors. The concentration-response relationship for all FDs were described by polynomial function models, being confirmed by Fisher variance (F-test). The% recoveries were in a range of 91.9-112.1%. Good method precision was observed, yielding relative standard deviations (RSDs) less than 4.9% for repeatability and 8.8% for intermediate precision. The limits of quantitation for the analytes ranged from 30.6 to 737.7μgkg-1. The MEPSR-CX/UHPLCCORTECS-PDA method revealed an effective and potential analytical tool for SCH authenticity control based on target analysis of FDs allowing a strict control and differentiation from other similar or adulterated products.
- Establishment of authenticity and typicality of sugarcane honey based on volatile profile and multivariate analysisPublication . Silva, Pedro; Freitas, Jorge; Silva, Catarina L.; Perestrelo, Rosa; Nunes, Fernando M.; Câmara, José S.Sugarcane honey (SCH) is a black syrup produced in Madeira Island widely known for their excellent quality being used in traditional pastry and confectionery. However, its notoriety has been affected by circumstances in which some producers do not guaranty the product quality. The purpose of this study was to establish, for the first time, the volatomic profile of SCH produced by certified and non-certified producers in order to define their authenticity and typicality as useful platform to ensure SCH safety, protect consumer interests and fight the continuous problems of food fraud and adulteration. Solid-phase microextraction in headspace mode (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was applied as high throughput approach for extraction, separation and identification of SCH volatile compounds. The extraction technique was optimized for nature of stationary phase, extraction temperature, extraction time, and validated according with IUPAC and AOAC guidelines. Different volatomic fingerprints for SCH from certified and non-certified producers were recognized, being identified up to 87 volatile organic compounds (VOCs) belonging to distinct chemical classes, mainly aldehydes, alcohols, ketones and furans. One-way ANOVA analysis showed the existence of 18 VOCs with statistically significant differences between volatile profiles from certified and non-certified producers. Principal component analysis (PCA) and linear discriminant analysis (LDA) differentiate and discriminate the samples from both type of producers. According to the obtained results, the followed strategy revealed an effective way to establish the authenticity and typicality of SCH, providing useful information to producers that might therefore be used to improve the SCH quality and a powerful platform to promote a European certification application.
- 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.