Polycyclic aromatic hydrocarbons (PAHs) are neutral compounds containing multiple aromatic fused rings that are present in fossil fuels and can be formed from the incomplete combustion of organic material. In recent years, it has been well documented that several PAHs can be potentially carcinogenic via exposure or ingestion.
In this application note, we analyze 16 PAHs by LC/CMS (EPA 610 Mix) on the EPA priority target list using the Advion expression Compact Mass Spectrometer (CMS) coupled with the Advion AVANT UHPLC system.
The Touch Express™ Open Port Sampling Interface (OPSI), is designed for simple sampling of solids, liquids and sample preparation tips and fibers. The novel ambient sampling technique was developed by Gary Van Berkel and Vilmos Kertesz, of Oak Ridge National Laboratory.
Paired with the electrospray ion source of the expression® Compact Mass Spectrometer, the product incorporates a low volume, open port of continuously swept solvent, flowing directly into the electrospray ion source of the mass spectrometer.
During this webinar you will:
Learn how any soluble material touching the port is analyzed by the expression® Compact Mass Spectrometer in just seconds.
Learn how the sample technique eliminates sample preparation and provides zero carry over.
Find fast analysis methods for solids, liquids and sample preparation tips and fibers.
Damien Ertz, Ulrick Søchting, Alice Gadea, Maryvonne Charrier, Roar S. Poulsen
The new genus and species Ducatina umbilicata is described from Îles Crozet and Îles Kerguelen. This lichen is characterized by an umbilicate thallus with a black verrucose lower surface and a greyish to dark olivaceous smooth upper surface having large verrucae, large semiimmersed cephalodia, semi-immersed apothecia with a prominent thalline margin, simple, mainly ellipsoid ascospores of 23–42Å~12–25 μm and the presence of unknown chemical compounds. Phylogenetic analyses using nuLSU and mtSSU sequences place Ducatina in the Trapeliaceae (Baeomycetales). The new taxon is closely related to Orceolina antarctica and O. kerguelensis, two other lichens endemic to these subantarctic islands, differing by its morphology and the lack of chemical compounds. Ducatina is the only genus in the Trapeliaceae to develop a large umbilicate thallus.
The HPLC/MS analysis was carried out using Advion Expression® CMS ESI.
Pierre Le Pogam, Aline Pillot, Françoise Lohezic-le Devehat, Anne-Cécile Le Lamer, Béatrice Legouin, Alice Gadea, Aurélie Sauvager, Damien Ertz, Joël Boustie
Thin-layer chromatography (TLC) still enjoys widespread popularity among lichenologists as one of the fastest and simplest analytical strategies, today remaining the primary method of assessing the secondary product content of lichens. The pitfalls associated with this approach are well known as TLC leads to characterizing compounds by comparison with standards rather than properly identifying them, which might lead to erroneous assignments, accounting for the long-held interest in hyphenating TLC with dedicated identification tools. As such, commercially available TLC/Mass Spectrometry (MS) interfaces can be easily connected to any brand of mass spectrometer without adjustments. The spots of interest are extracted from the TLC plate to retrieve mass spectrometric signals within one minute, thereby ensuring accurate identification of the chromatographed substances. The results of this hyphenated strategy for lichens are presented here by 1) describing the TLC migration and direct MS analysis of single lichen metabolites of various structural classes, 2) highlighting it through the chemical profiling of crude acetone extracts of a set of lichens of known chemical composition, and finally 3) applying it to a lichen of unknown profile, Usnea trachycarpa.
The TLC/MS analysis was carried out using Advion Expression® CMS + Plate Express.
Alba Noël,Solenn Ferron, Isabelle Rouaud,Nicolas Gouault, Jean-Pierre Hurvois, Sophie Tomasi
Actinobacteria are well known for their potential in biotechnology and their production of metabolites of interest. Lichens are a promising source of new bacterial strains, especially Actinobacteria, which afford a broad chemical diversity. In this context, the culture medium of the actinobacterium Nocardia ignorata, isolated from the terrestrial lichen Collema auriforme, was studied. The strain was cultivated in a BioFlo 115 bioreactor, and the culture medium was extracted using an XAD7HP resin. Five known diketopiperazines: cyclo (l-Pro-l-OMet) (1), cyclo (l-Pro-l-Tyr) (2), cyclo (d-Pro-l-Tyr) (3), cyclo (l-Pro-l-Val) (4), cyclo (l-Pro-l-Leu) (5), and one auxin derivative: indole-carboxaldehyde (8) were isolated, along with two new brominated diketopiperazines: cyclo (d-Pro-l-Br-Tyr) (6) and cyclo (l-Pro-l-Br-Tyr) (7). Structure elucidation was performed using HRMS and 1D and 2D NMR analysis, and the synthesis of compounds 6 and 7 was carried out in order to confirm their structure.
The MS analysis was carried out using Advion Expression® CMS.
Martin Doert, Stephanie Krüger, Gertrud E. Morlock, Lothar W. Kroh
Ternary mixtures of lecithins, vitamin C and vitamin E are powerful antioxidants for the stabilization of polyunsaturated (n-3 fatty acid) oils. In this study, the chemistry of the antioxidant synergistic effect was investigated in ethyl linoleate (EL) containing α-tocopherol (α-Toc) or in linoleate rich vegetable oils at 110 °C using mixtures of phosphatidylethanolamine (PE) and either l-ascorbic acid (AA) or l-dehydroascorbic acid (DHA). The highest stabilization effects in EL were similar in both systems and were found in the molar mixtures of PE and AA or DHA. The thermal formation of reaction products between PE and AA (PE–AA) or DHA (PE–DHA) were investigated by HPTLC/ESI-MS. When α-tocopherylquinone (α-TQ) was used instead of α-Toc, nearly the same antioxidant effect was observed in the EL system. It was shown that molar mixtures of PE and AA, or PE and DHA, can regenerate α-TQ to α-Toc at elevated temperatures. PE–AA was synthesized and tested as antioxidants in EL containing α-Toc and in vegetable oils at room temperature. An improved stabilization was observed with the synthesized derivative compared to the physical mixture of the compounds, which demonstrated that PE–AA is a potential new antioxidant. A mechanism for the synergistic action between PE, AA and α-Toc through an acid-catalysed regeneration of α-TQ is suggested. PE–AA is an active apolar antioxidant, which is involved in the reduction of α-TQ.
The MS analysis was carried out using Advion Expression® CMS TLC and ESI.
Alice Gadea, Pierre Le Pogam, Grichka Biver, Joël Boustie, Anne-Cécile Le Lamer, Le Dévéhat Françoise, Maryvonne Charrier
Notodiscus hookeri is the only representative of terrestrial gastropods on Possession Island and exclusively feeds on lichens. The known toxicity of various lichen metabolites to plant-eating invertebrates led us to propose that N. hookeri evolved means to protect itself from their adverse effects. To validate this assumption, the current study focused on the consumption of two lichen species: Usnea taylorii and Pseudocyphellaria crocata. A controlled feeding experiment was designed to understand how the snail copes with the unpalatable and/or toxic compounds produced by these lichen species. The occurrence of two snail ecophenotypes, represented by a mineral shell and an organic shell, led to address the question of a metabolic response specific to the phenotype. Snails were fed for two months with one of these lichens and the chemical profiles of biological samples of N. hookeri (i.e., crop, digestive gland, intestine, and feces) were established by HPLC-DAD-MS and compared to that of the lichens. N. hookeri appears as a generalist lichen feeder able to consume toxic metabolite-containing lichens, independently of the ecophenotype. The digestive gland did not sequester lichen metabolites. The snail metabolism might be based on four non-exclusive processes according to the concerned metabolites (avoidance, passive transport, hydrolysis, and excretion).
The LC/MS analysis was carried out using Advion Expression® CMS ESI.
Explosive and Pollutant Nitro Aromatics (epNACs) like 2,4,6-trinitrophenol (TNP) has been detected from various surface water specimens by luminescent Schiff base Organic Frameworks (SOFs) by fluorometric method. Fluorescence intensity of the receptor SOFs have been quenched in presence of TNP due to RET and ICT, which has been confirmed through solid and solution level spectroscopic studies like FT-IR, 1H-NMR, fluorescence titration. Modern DFT (DFT-D3) calculations of the possible host guest conformers have been performed for exploration of plausible route of interaction between receptor and epNACs. The outcome of theoretical calculations is in line with experimental findings where TNP and receptor conformation mimic parallel displaced type π- π interaction. TD-DFT has been executed with both receptor and receptor ···TNP adduct, the fluorescence quenching is in line with experimental outcome. Limit of TNP detection has been found as low as 5 μM with 2.97×104 M-1 as binding constant. In real time stepping, TNP as mutagenic agent for aquatic life has been detected inside prokaryotic cells like candidia albicans in ppm level.
The MS analysis was carried out using Advion Expression® CMS ESI.
Shared live at the 254th ACS National Meeting in Washington, D.C. –
John Matson, Ph. D., Matson Research Group on Macromolecular and Supramolecular Chemistry, Assistant Professor, Virginia Tech.
Listen to the recorded workshop session highlighting the role of H2S in the human body and how compact mass spectrometry is used to assay peptides via direct injection for reaction monitoring, and coupled with HPLC for purification.
Advion Interchim Scientific’s range of AVANT®, high performance, liquid chromatography systems can be used standalone with UV and UV/Vis detector options, or with the expression® compact mass spectrometer to provide seamlessly integrated LC/CMS under the full control of Advion Interchim Scientific’s simple, intuitive Mass Express software suite.
Modular, stackable design, with many options, provides custom solutions for both HPLC and UHPLC needs. From the simplest manual injection HPLC to a fully automated, streamlined UHPLC system and everything in-between, the AVANT® series can be configured to fit your analytical requirements and your budget.
