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Analysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MS

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dc.contributor.authorPaíga, Paula
dc.contributor.authorRodrigues, Manuela J.E.
dc.contributor.authorCorreia, Manuela
dc.contributor.authorAmaral, Joana S.
dc.contributor.authorOliveira, M. Beatriz P.P.
dc.contributor.authorDelerue-Matos, Cristina
dc.date.accessioned2017-01-26T12:32:51Z
dc.date.embargo2117
dc.date.issued2016
dc.description.abstractA method based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was successfully developed and validated for the analysis of 26 pharmaceutical compounds belonging to different therapeutic classes (anorexics, stimulants, anxiolytics, antidepressants and laxatives), which are all prone to be illegally added into weight-loss plant food supplements (PFS) for their pharmacological activity. Internal standard calibration with six isotopically labelled compounds rendered good linearity in the range of 5 to 1000 μg/l, depending on the compound, and good sensitivity with limits of quantification in the range of 0.02–9.80 μg/l. Recoveries were assessed for all the 16 samples analysed and were found between 70% and 120% for over 90% of the analytes. The average recovery value was 90.8%, for the different studied matrices (liquids, liquid ampoules, tablets and capsules), with RSD values lower than 10% for all forms. The changes introduced to the QuEChERS procedure maintained the good performance characteristics of the extraction methodwhile preserving the chromatographic systemfor the introduction of unwanted matrix compounds. Synephrinewas the only compound detected and quantified in one sample, but at a very lowconcentration (768 μg/l) and its presence may be due to the plant extracts used in the formulation, as synephrine is known to be a natural constituent of Citrus aurantium amara. Despite none of the 16 evaluated sampleswere found to be adulterated by the illegal addition of the drugs included in this work, the developed methodology can be very useful for monitoring the adulteration of weight-loss PFS.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.doihttp://dx.doi.org/10.1016/j.ejps.2016.12.024pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.22/9435
dc.language.isoengpt_PT
dc.publisherElsevierpt_PT
dc.relation.ispartofseriesEuropean Journal of Pharmaceutical Sciences;Vol. 99
dc.relation.publisherversionhttp://www.sciencedirect.com/science/article/pii/S0928098716305644pt_PT
dc.subjectPlant food supplementspt_PT
dc.subjectPharmaceuticalspt_PT
dc.subjectQuEChERSpt_PT
dc.subjectUltra-high performance liquid chromatographypt_PT
dc.subjectMass spectrometrypt_PT
dc.titleAnalysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MSpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.titleEuropean Journal of Pharmaceutical Sciencespt_PT
oaire.citation.volume99pt_PT
person.familyNamePaíga
person.familyNameDelerue-Matos
person.givenNamePaula
person.givenNameCristina
person.identifier1668889
person.identifier.ciencia-id331A-5D6A-D3C8
person.identifier.ciencia-id9A1A-43FB-5C27
person.identifier.orcid0000-0002-9593-1355
person.identifier.orcid0000-0002-3924-776X
person.identifier.ridQ-4930-2018
person.identifier.ridD-4990-2013
person.identifier.scopus-author-id6506638953
person.identifier.scopus-author-id6603741848
rcaap.rightsclosedAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublication4a0677dc-0b54-4831-aa9a-4a73f0df911d
relation.isAuthorOfPublication09f6a7bd-2f15-42b0-adc5-04bd22210519
relation.isAuthorOfPublication.latestForDiscovery4a0677dc-0b54-4831-aa9a-4a73f0df911d

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