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Despite the widespread use of artichoke-based food supplements for obesity control (FSOC), studies on evaluation of the quality/authenticity of these commercial products are scarce. To that aim, a new multi-analytical strategy, based on the use of gas chromatography coupled to mass spectrometry (GC-MS) and high performance liquid chromatography coupled to ultraviolet and mass spectrometry detection (HPLC-UV-MS), in combination with chemometrics, has been developed. Twenty-one artichoke FSOC and different bract and leaf extracts (used as reference samples) were analysed. Sugars, inositols, caffeoylquinic acids, dicaffeoylquinic acids, flavonoids and their glycosides were detected in reference samples and in most artichoke FSOC. Low concentrations of bioactives, and the presence of other compounds probably related to heat treatment during manufacturing (difructosyl anhydrides, 3-deoxyglucosone), or to the addition of caloric additives (maltose, maltotriose) or non-declared plants (e.g. pinitol, disaccharides, silybin derivatives) were also detected in some FSOC by either GC-MS or HPLC-UV-MS. Application of Principal Component Analysis to the combined GC-MS + HPLC-UV data matrix, proved that this multi-analytical strategy provides advantages over single analytical techniques for the detection of the wide variety of fraudulent practices affecting authenticity of artichoke FSOC and for assessment of their quality., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021. Published by Elsevier B.V.)

Considering the interest in the bioactive properties of saffron (Crocus sativus L.), as well as its limited production and high price, saffron-based food supplements (SFS) are highly susceptible to adulteration. However, their complex composition and the wide variety of potential fraudulent practices make the comprehensive assessment of SFS quality a challenging task that has been scarcely addressed. To that aim, a new multianalytical strategy based on gas chromatography coupled to mass spectrometry (GC-MS) and liquid chromatography with diode array detection coupled to mass spectrometry (HPLC-DAD-MS) was developed and validated in order to detect different frauds affecting SFS. Dried saffron stigmas and a commercial standardized saffron extract (affron®) were selected as reference samples (RS) to obtain an authenticity profile, which was further used to evaluate the quality of 17 SFS. Up to 17 crocins and crocetins, 5 kaempferol glycosides, picrocrocin (determined for the first time by GC-MS), safranal, furanone and isophorone-related compounds were determined in RS. Safranal and crocins were identified in all SFS except for one sample. However, discrepancies with the content declared were detected in 65% of the cases. Moreover, this multianalytical methodology also allowed identifying undeclared additives and the non-declared addition of vegetable sources other than saffron. [ABSTRACT FROM AUTHOR]

Food supplements based on saffron (Crocus sativus L.) dried stigma extracts are widely consumed due to their multiple bioactive properties. Saffron extract (SE) standardization is of crucial importance, as it determines the reproducibility of the product quality and is essential for the evaluation of its bioactive effect and safety. Although SEs are commonly standardized considering their safranal content, the lack of specificity of the official methods may give inaccurate measurements. In addition to the development of more precise methodologies, the evaluation of alternative saffron components, such as crocins and picrocrocin, for standardization purposes would also be of interest. Thus, in this study, qualitative and quantitative information regarding picrocrocin and crocin isomers of different commercial saffron extracts was first obtained by a validated methodology using liquid chromatography (HPLC) coupled to diode array (DAD) and mass spectrometer (MS) detectors. Principal component analysis (PCA) was applied to gain insight into the compositional variability and natural grouping of SE. These studies suggested the potential use of the relative content of crocin isomers and trans-/cis-crocins and trans-4 GG/picrocrocin ratios as novel criteria for SE standardization. Their reproducibility and stability under controlled storage conditions for 36 months was demonstrated in a commercial standardized SE (affron®). [ABSTRACT FROM AUTHOR]

[Display omitted] • A GC–MS method was developed and validated for hydroxycitric acid (HCA) analysis. • Derivatization reagents and conditions were crucial for the GC–MS analysis of HCA. • HCA content of 12 Garcinia cambogia food supplements (GFS) was determined. • 42% of the samples did not comply with the HCA content declared on the label. • This method was useful to analyze HCA and detect frauds in GFS. Garcinia gummi-gutta based food supplements (GFS) are widely commercialized due to their antiobesity activity, which has been mainly attributed to their high content in (−)-hydroxycitric acid [(−)-HCA]. In order to overcome the limitations related to selectivity and sensitivity of the HPLC-UV methods usually employed for the analysis of this compound, a GC–MS method was fully developed for the first time and validated. Water with 0.1 % formic acid was used for the solubilization of (−)-HCA stabilized in the form of salt in GFS. After a drying step, different derivatization solvents were tested and only trifluoroacetic acid (TFA) allowed the complete dissolution of (−)-HCA. Regarding silylation, the best results were obtained by cold dropwise addition of hexamethyldisilazane and subsequent heating at 45 °C for 90 min. After optimizing the chromatographic conditions, the stability of derivatives for 1 month was also assessed. This new methodology was also applied to determine the (−)-HCA content of 12 commercial GFS. Experimental values ranged from 0.86 to 61%. Forty-two percent of the analyzed samples did not meet the (−)-HCA content declared on the label and 2 GFS showed HCA concentrations lower than 10% (0.86 and 6.0%), which puts into question their effectiveness in regulating obesity. One advantage of this new methodology is that it allows the qualitative and quantitative analysis of (−)-HCA in GFS without coelutions with other interfering compounds and it avoids the solubility problems presented by HCA salts. Moreover, the coupling of GC to MS provides more reliable identification of compounds present in GFS. [ABSTRACT FROM AUTHOR]