Browsing by Author "Correia, Manuela"
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- Adulteration of Brain Health (Cognitive, Mood, and Sleep Enhancement) Food Supplements by the Addition of Pharmaceutical Drugs: A Comprehensive Review of Analytical Approaches and TrendsPublication . Paiva, Rafael; Correia, Manuela; Delerue-Matos, Cristina; Amaral, Joana S.In recent years, the consumption of dietary supplements has grown worldwide, particularly in developed regions. However, this growing market has also become a prime target for adulteration practices, with some manufacturers illegally adding pharmaceuticals into plant-based food supplements (PFS) to enhance their effects. While extensive research has focused on detecting adulterant drugs in PFS tailored for improving sexual performance, weight loss, and muscle building, less attention has been given to supplements intended for mood enhancement, sleep aid, and cognitive function (nootropics). Nonetheless, recent reports indicate an increasing level of adulteration within this group of PFS. Therefore, this review aims at providing a comprehensive overview on the adulteration of PFS tailored for brain health, with a focus on the analytical techniques utilized for detection while also presenting data on consumption patterns and the prevalence of reported adulterants. Considering that the detection of such fraudulent practices primarily relies on chromatographic techniques coupled with mass spectrometry (MS), the developments in this field comprising either targeted or untargeted analysis of pharmaceutical adulterants are discussed.
- Analysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MSPublication . Paíga, Paula; Rodrigues, Manuela J.E.; Correia, Manuela; Amaral, Joana S.; Oliveira, Beatriz; Delerue-Matos, CristinaA 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 method while preserving the chromatographic system for the introduction of unwanted matrix compounds. Synephrine was the only compound detected and quantified in one sample, but at a very low concentration (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 samples were 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.
- Assessment of plant food supplements adulteration with psychopharmaceutical drugsPublication . Rodrigues, Manuela J.E.; Paíga, Paula; Santos, Lúcia H.M.L.M.; Amaral, Joana S.; Oliveira, Beatriz; Correia, Manuela; Delerue-Matos, CristinaThe purpose of this study was to compare three different extraction methods (two based on ethanol extraction and one on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERs) method) to assess the possible addition of psychopharmaceutical drugs (fluoxetine, sertraline, citalopram, venlafaxine, paroxetine, trazodone, and diazepam) as adulterants in St. John's wort (Hypericum perforatum) based plant food supplements (PFS). Methodology: Analysis was performed in a Nexera Ultra-High Performance Liquid Chromatograph (UHPLC) coupled to a triple-quadrupole mass spectrometer (LCMS-8030 Shimadzu) with an electrospray ionization source (ESI), operating in positive ion mode, using a Kinetex C18 fused core column (150 × 2.10 mm i.d.; 1.7 m) (Phenomenex). Multiple reaction monitoring mode (MRM) was selected and pharmaceuticals were quantified by internal standard calibration method. Calibration curves were constructed in the range 10 – 1000 g/L. The three different extraction methods were compared based on the analysis of spiked samples.
- Determination of psychopharmaceutical adulterants in plant food supplements using UHPLC-MS/MSPublication . Rodrigues, Manuela J.E.; Paíga, Paula; Santos, Lúcia H.M.L.M.; Amaral, Joana S.; Oliveira, Beatriz; Correia, Manuela; Delerue-Matos, CristinaIn the last decades, medicinal plants and derived products have become increasingly available on the EU market as components of formulations sold as plant food supplements (PFS). Such products are legally considered as foods under the Directive 2002/46/EC [l] and do not require any kind of authorization to be placed on the market. The legal responsibility for its safety relies on the business operators. Among the several issues that may aíFect the safety of PFS, adulterations including the addition of illegal substances represent an increasing public health concern. In this context, the adulteration by the addition of psychopharmaceuticals should be investigated. Chromatographic methods, especially LC, coupled to various detectors are commonly used for the detection of fraudulent addition of pharmaceuticals in complex mixtures such as PFS. Among them, LC-MS/MS provides accurate and sensitive detectíon ofthe target compounds [2]. The purpose of this study was to assess the presence of psychopharmaceutical adulterants namely, fluoxetine, sertraline, citalopram, venlafaxine, paroxetine, trazodone, and diazepam in St. Johns wort (Hypericum perforatum) based PFS since this plant and/or extracts are traditionally used for its antidepressive properties. Analysis was performed in a Nexera Ultra-High Performance Liquid Chromatograph coupled to a triple-quadrupole mass spectrometer (LCMS-8030 Shimadzu) with an electrospray ionization source (ESI), operating in positive ion mode, using a Kinetex C18 fused core column (150 x 2.10 mm i.d.; 1.7 [im) (Phenomenex). Multiple reaction monitoring mode (MRM) was selected and pharmaceuticals were quantified by internai standard calibration method. Prior to analysis PFS samples were extracted with methanol. The methodology was applied to a set of20 St. Johns wort based PFS commercially available in the Portuguese market.
- Monitoring of ochratoxin a exposure of the Portuguese population through a nationwide urine survey – Winter 2007Publication . Duarte, S.C.; Bento, J.M.V.; Pena, A.; Lino, C.M.; Delerue-Matos, Cristina; Oliva-Teles, T.; Morais, S.; Correia, Manuela; Oliveira, Beatriz; Alves, M. Rui; Pereira, J.A.Ochratoxin A (OTA) is a mycotoxin produced by a variety of fungi, such as Penicillium verrucosum and Aspergillium spp., which has been found to have a wide number of potentially deadly toxic effects, and can enter the human organism through a variety of means. It then finds its way into the bloodstream and, after a lengthy process, is eventually excreted through the urine. It can thus be detected in its original form not only in blood samples but also in this biological medium. As such, and in an attempt to evaluate the exposure of the Portuguese population to this mycotoxin, morning urine samples were collected during the Winter of 2007, from each of five geographically distinct Portuguese locations — Bragança, Porto, Coimbra, Alentejo, and Algarve — and subjected to extraction by immunoaffinity columns and to OTA quantification through liquid chromatography coupled with fluorescence detection. Prevalent incidence was higher than 95% with Coimbra being the exception (incidence of 73.3%). In nearly all locations, the OTA content of most samples was found to be above the limit of quantification (LOQ) of 0.008 ng/ml. Indeed, excluding Coimbra, with an OTA content level of 0.014 ng/ml, all regions featured content values over 0.021 ng/ml.
- Ochratoxin A contamination of bread – Portugal nationwide survey during winter 2007/2008.Publication . Duarte, S.C.; Bento, J.M.V.; Pena, A.; Lino, C.M.; Pereira, J.A.; Delerue-Matos, Cristina; Oliva-Teles, T.; Morais, S.; Correia, Manuela; Oliveira, BeatrizOchratoxin A (OTA) remains one of the most important mycotoxins known, due to its ubiquitous occurrence, wide range of susceptible food commodities and observed toxic effects, in both animals and humans. The reported toxic effects include carcinogenic, nephrotoxic, teratogenic, neurotoxic and immunotoxic.
- Ochratoxin A content in urine from Bragança and Alentejo: a compartive analysis (Winter 2007).Publication . Duarte, S.C.; Bento, J.M.V.; Pena, A.; Lino, C.M.; Pereira, J.A.; Delerue-Matos, Cristina; Oliva-Teles, T.; Morais, S.; Correia, Manuela; Oliveira, BeatrizOchratoxin A (OTA) is a mycotoxin which possesses a variety of toxic effects, including enzyme inhibition, immunosuppression, teratogenicity, nephrotoxicity, and carcinogenicity. It is produced by fungi for which foodstuffs such as beans, cereals, fruits, and seeds constitute an ideal growing media. It has proven itself at least partly resistant to food processing methods, meaning it is also present in derived products and thus finds its way into the human organism. Recent studies have suggested that, though OTA can be found in both plasma and urine – through which it is eliminated, though with great difficulty – the latter provides a better indication of OTA ingestion. Its collection procedure is also less invasive, and developments in analytical methodology allow an equally precise analysis.