Simultaneous Determination of 23 Pyrrolizidine and Tropane Alkaloids in Infusions from Dry Edible Flowers Using Optimized μSPEed® Microextraction Prior to Their Analysis by UHPLC-IT-MS/MS

dc.contributor.authorFernández-Pintor, Begoña
dc.contributor.authorMorante-Zarcero, Sonia
dc.contributor.authorSierra, Isabel
dc.date.accessioned2024-06-04T08:59:00Z
dc.date.available2024-06-04T08:59:00Z
dc.date.issued2024-06-01
dc.descriptionA miniaturized solid-phase extraction of two tropane alkaloids (TAs) and twenty-one pyrrolizidine alkaloids (PAs) from infusions of dry edible flowers using optimized µSPEed® technique was developed. The optimization of the µSPEed® methodology involved testing different cartridges and comparing various volumes and numbers of loading cycles. The final conditions allowed for a rapid extraction, taking only 3.5 min. This was achieved using a C18-ODS cartridge, conditioning with 100 µL of methanol (two cycles), loading 100 µL of the infusion sample (seven cycles), and eluting the analytes with 100 µL of methanol (two cycles). Prior to their analysis by UHPLC-IT-MS/MS, the extracts were evaporated and reconstituted in 100 µL of water (0.2% formic acid)/methanol (0.2% ammonia) 95:5 (v/v), allowing for a preconcentration factor of seven times. The methodology was successfully validated obtaining recoveries ranging between 87 and 97%, RSD of less than 12%, and MQL between 0.09 and 0.2 µg/L. The validated methodology was applied to twenty samples of edible flower infusions to evaluate the safety of these products. Two infusion samples obtained from Acmella oleracea and Viola tricolor were contaminated with 0.16 and 0.2 µg/L of scopolamine (TA), respectively, while the infusion of Citrus aurantium was contaminated with intermedine and lycopsamine (PAs) below the MQL.es
dc.description.abstractA miniaturized solid-phase extraction of two tropane alkaloids (TAs) and twenty-one pyrrolizidine alkaloids (PAs) from infusions of dry edible flowers using optimized µSPEed® technique was developed. The optimization of the µSPEed® methodology involved testing different cartridges and comparing various volumes and numbers of loading cycles. The final conditions allowed for a rapid extraction, taking only 3.5 min. This was achieved using a C18-ODS cartridge, conditioning with 100 µL of methanol (two cycles), loading 100 µL of the infusion sample (seven cycles), and eluting the analytes with 100 µL of methanol (two cycles). Prior to their analysis by UHPLC-IT-MS/MS, the extracts were evaporated and reconstituted in 100 µL of water (0.2% formic acid)/methanol (0.2% ammonia) 95:5 (v/v), allowing for a preconcentration factor of seven times. The methodology was successfully validated obtaining recoveries ranging between 87 and 97%, RSD of less than 12%, and MQL between 0.09 and 0.2 µg/L. The validated methodology was applied to twenty samples of edible flower infusions to evaluate the safety of these products. Two infusion samples obtained from Acmella oleracea and Viola tricolor were contaminated with 0.16 and 0.2 µg/L of scopolamine (TA), respectively, while the infusion of Citrus aurantium was contaminated with intermedine and lycopsamine (PAs) below the MQL.es
dc.identifier.citationFernández-Pintor, B.; Morante-Zarcero, S.; Sierra, I. Simultaneous Determination of 23 Pyrrolizidine and Tropane Alkaloids in Infusions from Dry Edible Flowers Using Optimized μSPEed® Microextraction Prior to Their Analysis by UHPLC-IT-MS/MS. Foods 2024, 13, 1740. https://doi.org/10.3390/foods13111740es
dc.identifier.doi10.3390/foods13111740es
dc.identifier.issn2304-8158 (online)
dc.identifier.urihttps://hdl.handle.net/10115/33339
dc.language.isoenges
dc.publisherMDPIes
dc.rightsAtribución 4.0 Internacional*
dc.rights.accessRightsinfo:eu-repo/semantics/openAccesses
dc.rights.urihttp://creativecommons.org/licenses/by/4.0/*
dc.subjectdry edible flowerses
dc.subjectinfusionses
dc.subjecttropane alkaloidses
dc.subjectpyrrolizidine alkaloidses
dc.subjectmicroextractiones
dc.subjectHPLC-MS/MSes
dc.titleSimultaneous Determination of 23 Pyrrolizidine and Tropane Alkaloids in Infusions from Dry Edible Flowers Using Optimized μSPEed® Microextraction Prior to Their Analysis by UHPLC-IT-MS/MSes
dc.typeinfo:eu-repo/semantics/articlees

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