Preliminary investigation of biogenic amines in type I sourdoughs produced at home and bakery level

10openInternationalItalian coauthor/editorDuring a survey for isolating sourdough lactic acid bacteria (LAB), 20 dough samples produced at the bakery level (BL) or home-made (HM) were collected. An enzyme-based colorimetric method revealed a total biogenic amines (BAs) concentration in the range 41.4–251.8 ppm for six (three BL and three HM) sourdoughs characterised by unpleasant odours. Eight BAs generally investigated in foods were identified and quantified from these six samples by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS). Only one HM sample contained almost all analysed BAs. Tryptamine was exclusively detected in HM sourdoughs (0.71–24.1 ppm). Putrescine, tryptamine, spermidine, and spermine were the only BAs detected in BL sourdoughs. MiSeq Illumina analysis was applied to study the total bacterial community of sourdoughs. LAB accounted from 67.89 to 92.17% of total bacterial diversity, and Levilactobacillus brevis was identified in all six sourdoughs. Leuconostoc, Pediococcus, and Weissella were also dominant. Plate counts detected neither the presence of Pseudomonas nor members of the Enterobacteriaceae family, and LAB levels were, on average, barely 5.89 Log CFU/g for BL, and 7.33 Log CFU/g for HM sourdoughs. Data suggested that the microorganisms mainly imputable of BAs formation in sourdough are members of the LAB communityopenMannino, Giuseppe; Cirlincione, Fortunato; Gaglio, Raimondo; Franciosi, Elena; Francesca, Nicola; Moschetti, Giancarlo; Asteggiano, Alberto; Medana, Claudio; Gentile, Carla; Settanni, LucaMannino, G.; Cirlincione, F.; Gaglio, R.; Franciosi, E.; Francesca, N.; Moschetti, G.; Asteggiano, A.; Medana, C.; Gentile, C.; Settanni, L

HPLC-HRMS global metabolomics approach for the diagnosis of "olive quick decline syndrome" markers in olive trees leaves

10openInternationalItalian coauthor/editorOlive quick decline syndrome (OQDS) is a multifactorial disease affecting olive plants. The onset of this economically devastating disease has been associated with a Gram-negative plant pathogen called Xylella fastidiosa (Xf). Liquid chromatography separation coupled to high-resolution mass spectrometry detection is one the most widely applied technologies in metabolomics, as it provides a blend of rapid, sensitive, and selective qualitative and quantitative analyses with the ability to identify metabolites. The purpose of this work is the development of a global metabolomics mass spectrometry assay able to identify OQDS molecular markers that could discriminate between healthy (HP) and infected (OP) olive tree leaves. Results obtained via multivariate analysis through an HPLC-ESI HRMS platform (LTQ-Orbitrap from Thermo Scientific) show a clear separation between HP and OP samples. Among the differentially expressed metabolites, 18 different organic compounds highly expressed in the OP group were annotated; results obtained by this metabolomic approach could be used as a fast and reliable method for the biochemical characterization of OQDS and to develop targeted MS approaches for OQDS detection by foliage analysisopenAsteggiano, A.; Franceschi, P.; Zorzi, M.; Aigotti, R.; Dal Bello, F.; Baldassarre, F.; Lops, F.; Carlucci, A.; Medana, C.; Ciccarella, G.Asteggiano, A.; Franceschi, P.; Zorzi, M.; Aigotti, R.; Dal Bello, F.; Baldassarre, F.; Lops, F.; Carlucci, A.; Medana, C.; Ciccarella, G

Development, Validation, and Application of a Simple and Rugged HPLC Method for Boswellic Acids for a Comparative Study of Their Abundance in Different Species of Boswellia Gum Resins

The resin of Boswellia plant species has been used since ancient times for its several bio-active curative effects. In modern times, extracts of this resin are still widely commercialized on the food supplements and nutraceuticals market. Nowadays the legislation on botanical extracts and the increasing demand for their safety and traceability are setting new standards for their chemical characterization. In this work we present an easy, feasible and rugged HPLC-UV-based approach for the quantitation of boswellic acids in food-supplement-grade resin extracts of Boswellia plant species. This method can be used for quality control purposes as well as for studying their differences in regional origin, years of harvesting and species-related differences. The method employs a C18 (3 × 150 mm, 3 µm) analytical HPLC column, and the separation is carried out through a gradient of acetonitrile/water with 0.1% formic acid. The method was validated following the ICH guidelines and used to quantitate different samples of commercial resin of Boswellia carteri and serrata together with other samples from unknown species. The six known boswellic acids were identified and quantified in all the analyzed samples. The results were used to build a multivariate model to graphically appreciate their difference through their clustering. The model was then augmented by adding further quantitation data for boswellic acids belonging to different species of Boswellia obtained by another scientific publications to increase the number of studied samples

Quali–Quantitative Characterization of Volatile and Non-Volatile Compounds in Protium heptaphyllum (Aubl.) Marchand Resin by GC–MS Validated Method, GC–FID and HPLC–HRMS2

Protium heptaphyllum (Aubl.) Marchand (PH) trees are endemic to the tropical region of South America, mostly Brazil. Antibacterial, antinociceptive, anti-inflammatory, anxiolytic, antidepressant and anti-hyperlipidemic/anti-hypercholesterolemic effects were reported for its resinous exudate Protiumheptaphyllum resin (PHR). This work aims to provide a qualitative and quantitative consistent chemical profiling of the major constituents of this resin and two extracts enriched in acid (acidic triterpene concentrated extract, ATCE) and neutral triterpenes (α and β-amyrin concentrated extract, AMCE). GC–MS/GC–FID was used for volatile terpene fraction, a validated GC–MS method was developed for quantification of neutral α and β-amyrin and HPLC–APCI HRMS2 was used for acidic triterpenes analysis. The chemical investigation reported 29 molecules, including 14 volatile terpenes, 6 neutral triterpenes and 11 acid triterpenes. The most abundant compounds were α-amyrin (251.28 g kg−1, 123.98 g kg−1 and 556.82 g kg−1 in PHR, ATCE and AMCE, respectively), β-amyrin (172.66 g kg−1, 95.39 g kg−1 and 385.58 g kg−1 in PHR, ATCE and AMCE, respectively), 3-oxo-tirucalla-7,24-dien-21-oic acid (80.64 g kg−1, 157.10 g kg−1 and 15.31 g kg−1 in PHR, ATCE and AMCE, respectively) and 3α-hydroxy-tirucalla-8,24-dien-21-oic acid (77.71 g kg−1, 130.40 g kg−1 and 11.64 g kg−1 in PHR, ATCE and AMCE, respectively). Results showed specific enrichment of acidic and neutral triterpenoids in the two respective extracts

Release of Selected Non-Intentionally Added Substances (NIAS) from PET Food Contact Materials: A New Online SPE-UHPLC-MS/MS Multiresidue Method

Food contact materials (FCMs) are an underestimated source of food chemical contaminants and a potentially relevant route of human exposure to chemicals that are harmful to the endocrine system. Foods and water are the main sources of exposure due to contact with the packaging materials, often of polymeric nature. European Regulation 10/2011 requires migration tests on FCMs and foodstuffs to evaluate the presence of listed substances (authorized monomers and additives) and non-intentionally added substances (NIAS) not listed in the regulation and not subjected to restrictions. The tests are required to ensure the compliance of packaging materials for the contained foods. NIAS are a heterogeneous group of substances classified with a potential estrogenic or androgenic activity. Subsequently, the evaluation of the presence of these molecules in foods and water is significant. Here we present an online SPE/UHPLC-tandem MS method to quantify trace levels of NIAS in food simulants (A: aqueous 3% acetic acid; B: aqueous 20% ethanol) contained in PET preformed bottles. The use of online SPE reduces systemic errors thanks to the automation of the technique. For the developed analytical method, we evaluate the limit of detection (LOD), the limit of quantitation (LOQ), selectivity, RSD% and BIAS% for LLOQ for a total of twelve NIAS, including monomers, antioxidants, UV-filters and additives. LOD ranged between 0.002 µg/L for bisphenol S and 13.6 µg/L for 2,6-di-tert-butyl-4-methylphenol (BHT). LOQs are comprised between 0.01 µg/L for bisphenol S and 42.2 µg/L for BHT. The online-SPE/UHPLC-tandem MS method is applied to the food simulants contained in several types of PET packaging materials to evaluate the migration of the selected NIAS. The results show the presence (µg/L) of NIAS in the tested samples, underlining the need for a new regulation for these potentially toxic molecules