Search results for: isotope ratio mass spectrometry

Authors: Yao-Te Yen, Chao-Hsin Cheng, Meng-Shun Huang, Shan-Zong Cyue

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'Poppy-seed defense' has been a serious problem all over the world, that is because the opiates metabolites in urine are difficult to distinguish where they come from precisely. In this research, a powerful analytic method has been developed to trace the opiates metabolites in urine by Gas-Chromatography Isotope Ratio Mass Spectrometry (GC-IRMS). In order to eliminate the interference of synthesis to heroin or metabolism through human body, opiates metabolites in urine and sized heroin were hydrolyzed to morphine. Morphine is the key compound for tracing between opiates metabolites and seized heroin in this research. By matching δ13C and δ15N values through morphine, it is successful to distinguish the opiates metabolites coming from heroin or medicine. We tested seven heroin abuser’s metabolites and seized heroin in crime sites, the result showed that opiates metabolites coming from seized heroin, the variation of δ13C and δ15N for morphine are within 0.2 and 2.5‰, respectively. The variation of δ13C and δ15N for morphine are reasonable with the result of matrix match experiments. Above all, the uncertainty of 'Poppy-seed defense' can be solved easily by this analytic method, it provides the direct evidence for judge to make accurate conviction without hesitation.

Keywords: poppy-seed defense, heroin, opiates metabolites, isotope ratio mass spectrometry

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Authors: Efthimios Kokkotos, Kostakis Marios, Beis Alexandros, Angelos Patakas, Antonios Avgeris, Vassilios Triantafyllidis

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H, C, and O stable isotope ratios were measured in different olive oils and table olives originating from different regions of Greece. In particular, the stable isotope ratios of different olive oils produced in the Lakonia region (Peloponesse – South Greece) from different varieties, i.e., cvs ‘Athinolia’ and ‘koroneiki’, were determined. Additionally, stable isotope ratios were also measured in different table olives (cvs ‘koroneiki’ and ‘kalamon’) produced in the same region (Messinia). The aim of this study was to provide sufficient isotope ratio data regarding each variety and region of origin that could be used in discriminative studies of oil olives and table olives produced by different varieties in other regions. In total, 97 samples of olive oil (cv ‘Athinolia’ and ‘koroneiki’) and 67 samples of table olives (cvs ‘kalmon’ and ‘koroneiki’) collected during two consecutive sampling periods (2021-2022 and 2022-2023) were measured. The C, H, and O isotope ratios were measured using Isotope Ratio Mass Spectrometry (IRMS), and the results obtained were analyzed using chemometric techniques. The measurements of the isotope ratio analyses were expressed in permille (‰) using the delta δ notation (δ=Rsample/Rstandard-1, where Rsample and Rstandardis represent the isotope ratio of sample and standard). Results indicate that stable isotope ratios of C, H, and O ranged between -28,5+0,45‰, -142,83+2,82‰, 25,86+0,56‰ and -29,78+0,71‰, -143,62+1,4‰, 26,32+0,55‰ in olive oils produced in Lakonia region from ‘Athinolia’ and ‘koroneiki ‘varieties, respectively. The C, H, and O values from table olives originated from Messinia region were -28,58+0,63‰, -138,09+3,27‰, 25,45+0,62‰ and -29,41+0,59‰,-137,67+1,15‰, 24,37+0,6‰ for ‘Kalamon’ and ‘koroneiki’ olives respectively. Acknowledgments: This research has been co-financed by the European Regional Development Fund of the European Union and Greek national funds through the Operational Program Competitiveness, Entrepreneurship and Innovation, under the call RESEARCH—CREATE—INNOVATE (Project code: T2EDK-02637; MIS 5075094, Title: ‘Innovative Methodological Tools for Traceability, Certification and Authenticity Assessment of Olive Oil and Olives’).

Keywords: olive oil, table olives, Isotope ratio, IRMS, geographical origin

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Authors: Anna-Akrivi Thomatou, Anastasios Zotos, Eleni C. Mazarakioti, Efthimios Kokkotos, Achilleas Kontogeorgos, Athanasios Ladavos, Angelos Patakas

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It is well known that accurate determination of geographic origin to confront mislabeling and adulteration of foods is considered as a critical issue worldwide not only for the consumers, but also for producers and industries. Among agricultural products, rice (Oryza sativa L.) is the world’s third largest crop, providing food for more than half of the world’s population. Consequently, the quality and safety of rice products play an important role in people’s life and health. Despite the fact that rice is predominantly produced in Asian countries, rice cultivation in Greece is of significant importance, contributing to national agricultural sector income. More than 25,000 acres are cultivated in Greece, while rice exports to other countries consist the 0,5% of the global rice trade. Although several techniques are available in order to provide information about the geographical origin of rice, little data exist regarding the ability of these methodologies to discriminate rice production from Greece. Thus, the aim of this study is the comparative evaluation of stable isotope ratio methodology regarding its discriminative ability for geographical origin determination of rice samples produced in Greece compared to those from three other Asian countries namely Korea, China and Philippines. In total eighty (80) samples were collected from selected fields of Central Macedonia (Greece), during October of 2021. The light element (C, N, S) isotope ratios were measured using Isotope Ratio Mass Spectrometry (IRMS) and the results obtained were analyzed using chemometric techniques, including principal components analysis (PCA). Results indicated that the 𝜹 15N and 𝜹 34S values of rice produced in Greece were more markedly influenced by geographical origin compared to the 𝜹 13C. In particular, 𝜹 34S values in rice originating from Greece was -1.98 ± 1.71 compared to 2.10 ± 1.87, 4.41 ± 0.88 and 9.02 ± 0.75 for Korea, China and Philippines respectively. Among stable isotope ratios studied, values of 𝜹 34S seem to be the more appropriate isotope marker to discriminate rice geographic origin between the studied areas. These results imply the significant capability of stable isotope ratio methodology for effective geographical origin discrimination of rice, providing a valuable insight into the control of improper or fraudulent labeling. Acknowledgement: This research has been financed by the Public Investment Programme/General Secretariat for Research and Innovation, under the call “YPOERGO 3, code 2018SE01300000: project title: ‘Elaboration and implementation of methodology for authenticity and geographical origin assessment of agricultural products.

Keywords: geographical origin, authenticity, rice, isotope ratio mass spectrometry

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Authors: Shima Behkami, Nor Shahirul Umirah Idris, Sharifuddin Md. Zain, Kah Hin Low, Mehrdad Gholami, Nima A. Behkami, Ahmad Firdaus Kamaruddin

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In this work, Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Isotopic Ratio Mass Spectrometry (IRMS) and Ultrasound Milko Tester were used to study milk samples obtained from various geographical locations in Malaysia. ICP-MS was used to determine the concentration of trace elements in milk, water and soil samples obtained from seven dairy farms at different geographical locations in peninsular Malaysia. IRMS was used to analyze the milk samples for isotopic ratios of δ13C, 15N and 18O. Nutritional parameters in the milk samples were determined using an ultrasound milko tester. Data obtained from these measurements were evaluated by Principal Component Analysis (PCA) and Hierarchical Analysis (HA) as a preliminary step in determining geographical origin of these milk samples. It is observed that the isotopic ratios and a number of the nutritional parameters are responsible for the discrimination of the samples. It was also observed that it is possible to determine the geographical origin of these milk samples solely by the isotopic ratios of δ13C, 15N and 18O. The accuracy of the geographical discrimination is demonstrated when several milk samples from a milk factory taken from one of the regions under study were appropriately assigned to the correct PCA cluster.

Keywords: inductively coupled plasma mass spectroscopy ICP-MS, isotope ratio mass spectroscopy IRMS, ultrasound, principal component analysis, hierarchical analysis, geographical origin, milk

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Authors: Bakhtishod Matmuratov, Sakhiba Madraximova, Rakhmat Esanov, Alimjan Matchanov

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Studies have been performed to obtain complexes of glycyrrhizic acid and kinetins in a 2:1 ratio. The complex of glycyrrhizic acid and kinetins in a 2:1 ratio was considered evidence of the formation of a molecular complex by determining the molecular masses using chromato-mass spectroscopy and analyzing the IR spectra.

Keywords: monoammonium salt of glycyrrhizic acid, glycyrrhizic acid, supramolecular complex, isomolar series, IR spectroscopy

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Authors: M. Tassi, E. Dotsika, P. Karalis, A. Trantalidou, A. Mazarakis Ainian

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The Kythnos Island in Greece is of particular archaeological interest, as it has been inhabited from the 12th BC until the 7th AD. From island excavations, numerous faunal and human skeletal remains have been recovered. This work is the first attempt at the paleoenvironmental reconstruction of the island via stable isotope analysis. Specifically, we perform 13C and 18O isotope analysis in faunal bone apatite in order to investigate the climate conditions that prevailed in the area. Additionally, we conduct 13C and 15N isotope analysis in faunal bone collagen, which will constitute the baseline for the subsequent diet reconstruction of the ancient Kythnos population.

Keywords: stable isotopes analysis, bone collagen stable isotope analysis, bone apatite stable isotope analysis, paleodiet, palaeoclimate

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Authors: Silvia Portarena, Chiara Anselmi, Chiara Baldacchini, Enrico Brugnoli

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Extra virgin olive oil (EVOO) is a complex matrix mainly composed by fatty acid and other minor compounds, among which carotenoids are well known for their antioxidative function that is a key mechanism of protection against cancer, cardiovascular diseases, and macular degeneration in humans. EVOO composition in terms of such constituents is generally the result of a complex combination of genetic, agronomical and environmental factors. To selectively improve the quality of EVOOs, the role of each factor on its biochemical composition need to be investigated. By selecting fruits from four different cultivars similarly grown and harvested, it was demonstrated that Raman spectroscopy, combined with chemometric analysis, is able to discriminate the different cultivars, also as a function of the harvest date, based on the relative content and composition of fatty acid and carotenoids. In particular, a correct classification up to 94.4% of samples, according to the cultivar and the maturation stage, was obtained. Moreover, by using gas chromatography and high-performance liquid chromatography as reference techniques, the Raman spectral features further allowed to build models, based on partial least squares regression, that were able to predict the relative amount of the main fatty acids and the main carotenoids in EVOO, with high coefficients of determination. Besides genetic factors, climatic parameters, such as light exposition, distance from the sea, temperature, and amount of precipitations could have a strong influence on EVOO composition of both major and minor compounds. This suggests that the Raman spectra could act as a specific fingerprint for the geographical discrimination and authentication of EVOO. To understand the influence of environment on EVOO Raman spectra, samples from seven regions along the Italian coasts were selected and analyzed. In particular, it was used a dual approach combining Raman spectroscopy and isotope ratio mass spectrometry (IRMS) with principal component and linear discriminant analysis. A correct classification of 82% EVOO based on their regional geographical origin was obtained. Raman spectra were obtained by Super Labram spectrometer equipped with an Argon laser (514.5 nm wavelenght). Analyses of stable isotope content ratio were performed using an isotope ratio mass spectrometer connected to an elemental analyzer and to a pyrolysis system. These studies demonstrate that RR spectroscopy is a valuable and useful technique for the analysis of EVOO. In combination with statistical analysis, it makes possible the assessment of specific samples’ content and allows for classifying oils according to their geographical and varietal origin.

Keywords: authentication, chemometrics, olive oil, raman spectroscopy

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Authors: Hyunchul Oh

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One of the challenges in modern separation science and technology is the separation of hydrogen isotopes mixtures since D2 and H2 consist of almost identical size, shape and thermodynamic properties. Recently, quantum sieving of isotopes by confinement in narrow space has been proposed as an alternative technique. Despite many theoretical suggestions, however, it has been difficult to discover a feasible microporous material up to now. Among various porous materials, the novel class of microporous framework materials (COFs, ZIFs and MOFs) is considered as a promising material class for isotope sieving due to ultra-high porosity and uniform pore size which can be tailored. Hence, we investigate experimentally the fundamental correlation between D2/H2 molar ratio and pore size at optimized operating conditions by using different ultramicroporous frameworks. The D2/H2 molar ratio is strongly depending on pore size, pressure and temperature. An experimentally determined optimum pore diameter for quantum sieving lies between 3.0 and 3.4 Å which can be an important guideline for designing and developing feasible microporous frameworks for isotope separation. Afterwards, we report a novel strategy for efficient hydrogen isotope separation at technologically relevant operating pressure through the development of quantum sieving exploited by the pore aperture engineering. The strategy involves installation of flexible components in the pores of the framework to tune the pore surface.

Keywords: gas adsorption, hydrogen isotope, metal organic frameworks(MOFs), quantum sieving

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Authors: Mehdi Ghanavati

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The Effects of salinity level and duration on carbon isotope discrimination (Δ) of Matricaria chamomilla and Matricaria aurea were evaluated. Four ecotypes of M. chamomilla and four ecotypes of M. aurea were grown at different NaCl concentrations (control, 6, 12 and 18 dS/m) in sand culture condition. Carbon isotope discrimination (Δ) varied significantly (p<0.001) among ecotypes. The amount of carbon isotope discrimination (Δ) increased in first salinity level (6 dS/m), but in other levels (12 and 18 dS/m) it did not increase. Stages of salinity treatments (two stages: first from seedling stage until the end of the experiment and second stage of stress exertion began at stem elongation and seedlings emergence from rosette stage to harvest) had not a significant difference. Study of two spices of chamomile showed the M. aurea had a higher amount of carbon isotope discrimination (Δ) (22.9%) than M. chamomilla (22.48%).

Keywords: salinity, carbon isotope discrimination, Matricaria chamomilla, Matricaria aurea

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Authors: Haiyang Su, Kun Qian

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We developed a novel plasmonic matrix assisted laser desorption/ionization mass spectrometry (MALDI MS) approach to detect small nutrients and toxin in complex biological emulsion samples. We used silver nanoshells (SiO₂@Ag) with optimized structures as matrices and achieved direct analysis of ~6 nL of human breast milk without any enrichment or separation. We performed identification and quantitation of small nutrients and toxins with limit-of-detection down to 0.4 pmol (for melamine) and reaction time shortened to minutes, superior to the conventional biochemical methods currently in use. Our approach contributed to the near-future application of MALDI MS in a broad field and personalized design of plasmonic materials for real case bio-analysis.

Keywords: plasmonic materials, laser desorption/ionization, mass spectrometry, small nutrients, toxins

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Authors: Abanoub Mikhael, Darryl Hardie, Derek Smith, Helena Petrosova, Robert Ernst, David Goodlett

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Lipopolysaccharide (LPS) is a hallmark virulence factor of Gram-negative bacteria. It is a complex, structurally het- erogeneous mixture due to variations in number, type, and position of its simplest units: fatty acids and monosaccharides. Thus, LPS structural characterization by traditional mass spectrometry (MS) methods is challenging. Here, we describe the benefits of field asymmetric ion mobility spectrometry (FAIMS) for analysis of intact R-type lipopolysaccharide complex mixture (lipooligo- saccharide; LOS). Structural characterization was performed using Escherichia coli J5 (Rc mutant) LOS, a TLR4 agonist widely used in glycoconjugate vaccine research. FAIMS gas phase fractionation improved the (S/N) ratio and number of detected LOS species. Additionally, FAIMS allowed the separation of overlapping isobars facilitating their tandem MS characterization and un- equivocal structural assignments. In addition to FAIMS gas phase fractionation benefits, extra sorting of the structurally related LOS molecules was further accomplished using Kendrick mass defect (KMD) plots. Notably, a custom KMD base unit of [Na-H] created a highly organized KMD plot that allowed identification of interesting and novel structural differences across the different LOS ion families, i.e., ions with different acylation degrees, oligosaccharides composition, and chemical modifications. Defining the composition of a single LOS ion by tandem MS along with the organized KMD plot structural network was sufficient to deduce the composition of 181 LOS species out of 321 species present in the mixture. The combination of FAIMS and KMD plots allowed in-depth characterization of the complex LOS mixture and uncovered a wealth of novel information about its structural variations.

Keywords: lipopolysaccharide, ion mobility MS, Kendrick mass defect, Tandem mass spectrometry

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Authors: Madrakhimova Sakhiba, Matmurotov Bakhtishod, Boltaboyava Zilola, Matchanov Alimjan

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Analyzing the chemical composition of locally consumed food products is one of the urgent problems in the health sector today. Taking this into account, it analyzed the microelement content of Cydonia oblonga Miller (COM) fruit growing in the Republic of Uzbekistan using the ISP MS inductively coupled mass spectrometry method. fruits brought to a constant mass in the analysis were mineralized in a mixture of nitric acid-HNO₃ and hydrogen peroxide-H₂O₂ in a ratio of 3:2. The mineralized extract was diluted to 50 milliliters with double-distilled water and analyzed. The results of the analysis showed that the fruit is rich in micronutrients necessary for the human body, especially potassium-K and phosphorus-P among macroelements, Strontium-Sr and barium-Ba from microelements are more than other microelements. It was observed that the amount of trace elements contained in COM fruit does not exceed the permissible standards. Therefore, it can be recommended to eat this fruit every day to prevent various diseases that occur in the human body.

Keywords: cydonia oblonga miller, macroelement, microelement, inductively coupled mass spectrometry, hydrolysis, mineralization

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Authors: Hasan AL-Khshemawee, Manjree Agarwal, Xin Du, Yonglin Ren

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The possibility use of stable isotopes to study Medfly mating and life history were investigated in these experiments. 13C6 glucose was incorporated in the diet of the Mediterranean fruit fly Ceratitis capitata (Diptera: Tephidae). Treatments included labelling and unlabelled of either the media or adult sugar water. The measured started from egg hatching till the adults have died. After mating, the adults were analysed for 13C6 glucose ratio using Liquid chromatography-mass spectrometry LC-MS in two periods of time immediately and after three days of mating. Results showed that stable isotopes were used successfully for labelling Medfly in laboratory conditions, and there were significant differences between labelled and unlabelled treatment in eggs hatching, larval development, pupae emergence, survival of adults and mating behaviour. Labelling during larval development and combined labelling of larvae and adults resulted in detectable values. The label glucose in larvae stage did not effect on mating behaviour, however, the label glucose in adults’ stage was affected by mating behaviour. We recommended that it is possible to label adults of Mediterranean fruit fly C. capitata and detected the label after mating. This method offers good tools to study mating behaviour in Medfly and other types of insects and could be providing useful tools in genetic studies, sterile insect technique (SIT) or agricultural pest management. Also, we recommended using this technique in the field.

Keywords: stable isotope, sterile insect technique (SIT), medfly, mating behaviour

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Authors: Vijayalakshmi Marella, NageswaraRaoPilli

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This paper describes a simple, rapid and sensitive liquid chromatography / tandem mass spectrometry assay for the determination of montelukast in human plasma using montelukast d6 as an internal standard. Analyte and the internal standard were extracted from 50 µL of human plasma via solid phase extraction technique without evaporation, drying and reconstitution steps. The chromatographic separation was achieved on a C18 column by using a mixture of methanol and 5mM ammonium acetate (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min. Good linearity results were obtained during the entire course of validation. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more number of samples in short time, thus increasing the productivity. The proposed method was found to be applicable to clinical studies.

Keywords: Montelukast, tandem mass spectrometry, montelukast d6, FDA guidelines

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Authors: C. G. Mendez-Garcia, E. T. Romero-Guzman, H. Hernandez-Mendoza, C. Solis, E. Chavez-Lomeli, E. Chamizo, R. Garcia-Tenorio

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Plutonium is present in different concentrations in the environment and biological samples related to nuclear weapons testing, nuclear waste recycling and accidental discharges of nuclear plants. This radioisotope is considered the most radiotoxic substance, particularly when it enters the human body through inhalation of powders insoluble or aerosols. This is the main reason of the determination of the concentration of this radioisotope in the atmosphere. Besides that, the isotopic ratio of ²⁴⁰Pu/²³⁹Pu provides information about the origin of the source. PM₂.₅ sampling was carried out in the Metropolitan Zone of the Valley of Mexico (MZVM) from February 18th to March 17th in 2015 on quartz filter. There have been significant developments recently due to the establishment of new methods for sample preparation and accurate measurement to detect ultra trace levels as the plutonium is found in the environment. The accelerator mass spectrometry (AMS) is a technique that allows measuring levels of detection around of femtograms (10-15 g). The AMS determinations include the chemical isolation of Pu. The Pu separation involved an acidic digestion and a radiochemical purification using an anion exchange resin. Finally, the source is prepared, when Pu is pressed in the corresponding cathodes. According to the author's knowledge on these aerosols showed variations on the ²³⁵U/²³⁸U ratio of the natural value, suggesting that could be an anthropogenic source altering it. The determination of the concentration of the isotopes of Pu can be a useful tool in order the clarify this presence in the atmosphere. The first results showed a mean value of activity concentration of ²³⁹Pu of 280 nBq m⁻³ thus the ²⁴⁰Pu/²³⁹Pu was 0.025 corresponding to the weapon production source; these results corroborate that there is an anthropogenic influence that is increasing the concentration of radioactive material in PM₂.₅. According to the author's knowledge in Total Suspended Particles (TSP) have been reported activity concentrations of ²³⁹⁺²⁴⁰Pu around few tens of nBq m⁻³ and 0.17 of ²⁴⁰Pu/²³⁹Pu ratios. The preliminary results in MZVM show high activity concentrations of isotopes of Pu (40 and 700 nBq m⁻³) and low ²⁴⁰Pu/²³⁹Pu ratio than reported. These results are in the order of the activity concentrations of Pu in weapons-grade of high purity.

Keywords: aerosols, fallout, mass spectrometry, radiochemistry, tracer, ²⁴⁰Pu/²³⁹Pu ratio

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Authors: Tudor Deaconescu, Andrea Deaconescu

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The utilization of pneumatic muscles in the actuation of industrial systems is still in its early stages, hence studies on the constructive solutions which include an assessment of their functional performance with a focus on one of the most important characteristics-energy efficiency are required. A quality indicator that adequately reflects the energy efficiency of an actuator is the energy-to-mass ratio. This ratio is computed in the paper for various types and sizes of pneumatic muscles manufactured by Festo, and is subsequently compared to the similar ratios determined for two categories of pneumatic cylinders.

Keywords: pneumatic cylinders, pneumatic muscles, energy-to-mass ratio, muscle stroke

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Authors: Giovanni Meloni

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Recent results are presented from experiments carried out at the Advanced Light Source (ALS) at the Chemical Dynamics Beamline of Lawrence Berkeley National Laboratory using multiplexed synchrotron photoionization mass spectrometry. The reaction mixture and a buffer gas (He) are introduced through individually calibrated mass flow controllers into a quartz slow flow reactor held at constant pressure and temperature. The gaseous mixture effuses through a 650 μm pinhole into a 1.5 mm skimmer, forming a molecular beam that enters a differentially pumped ionizing chamber. The molecular beam is orthogonally intersected by a tunable synchrotron radiation produced by the ALS in the 8-11 eV energy range. Resultant ions are accelerated, collimated, and focused into an orthogonal time-of-flight mass spectrometer. Reaction species are identified by their mass-to-charge ratios and photoionization (PI) spectra. Comparison of experimental PI spectra with literature and/or simulated curves is routinely done to assure the identity of a given species. With the aid of electronic structure calculations, potential energy surface scans are performed, and Franck-Condon spectral simulations are obtained. Examples of these experiments are discussed, ranging from new intermediates characterization to reaction mechanisms elucidation and biofuels oxidation pathways identification.

Keywords: mass spectrometry, reaction intermediates, synchrotron photoionization, oxidation reactions

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Authors: Athena Nguyen, Rojin Belganeh

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Detecting and identifying differences in like polymer materials are key factors in failure and deformulation analysis, and reverse engineering. Pyrolysis-GC/MS is an easy solid sample introduction technique which expands the application areas of gas chromatography and mass spectrometry. The Micro furnace pyrolyzer is directly interfaced with the GC injector preventing any potential of cold spot, carryover, and cross contamination. In this presentation, the analysis of the differences in three polystyrene samples is demonstrated. Although the three samples look very similar by Evolve gas analysis (EGA) and Flash pyrolysis, there are indications of small levels of other materials. By performing Thermal desorption-GC/MS, the additive compounds between samples show the differences. EGA, flash pyrolysis, and thermal desorption analysis are the different modes of operations of the micro-furnace pyrolyzer enabling users to perform multiple analytical techniques.

Keywords: Gas chromatography/Mass spectrometry, pyrolysis, pyrolyzer, thermal desorption-GC/MS

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Authors: Ismael Zamora, Elisabeth Ortega, Tatiana Radchenko, Guillem Plasencia

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The structure elucidation based on Mass Spectra (MS) data of unknown substances is an unresolved problem that affects many different fields of application. The recent overview of software available for structure elucidation of small molecules has shown the demand for efficient computational tool that will be able to perform structure elucidation of unknown small molecules and peptides. We developed an algorithm for De-Novo fragment analysis based on MS data that proposes a set of scored and ranked structures that are compatible with the MS and MSMS spectra. Several different algorithms were developed depending on the initial set of fragments and the structure building processes. Also, in all cases, several scores for the final molecule ranking were computed. They were validated with small and middle databases (DB) with the eleven test set compounds. Similar results were obtained from any of the databases that contained the fragments of the expected compound. We presented an algorithm. Or De-Novo fragment analysis based on only mass spectrometry (MS) data only that proposed a set of scored/ranked structures that was validated on different types of databases and showed good results as proof of concept. Moreover, the solutions proposed by Mass Spectrometry were submitted to the prediction of NMR spectra in order to elucidate which of the proposed structures was compatible with the NMR spectra collected.

Keywords: De Novo, structure elucidation, mass spectrometry, NMR

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Authors: Reza Pashaei, Reda Dzingelevičienė

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An efficient, reliable, and sensitive multiclass analytical method has been expanded to simultaneously determine 15 human pharmaceutical residues in fish and shrimp tissue samples by ultra-high-performance liquid chromatography-tandem mass spectrometry. The investigated compounds comprise ten classes, namely analgesic, antibacterial, anticonvulsant, cardiovascular, fluoroquinolones, macrolides, nonsteroidal anti-inflammatory, penicillins, stimulant, and sulfonamide. A simple liquid extraction procedure based on 0.1% formic acid in methanol was developed. Chromatographic conditions were optimized, and mobile phase namely 0.1 % ammonium acetate (A), and acetonitrile (B): 0 – 2 min, 15% B; 2 – 5 min, linear to 95% B; 5 – 10 min, 95% B; and 10 – 12 min was obtained. Limits of detection and quantification ranged from 0.017 to 1.371 μg/kg and 0.051 to 4.113 μg/kg, respectively. Finally, amoxicillin, azithromycin, caffeine, carbamazepine, ciprofloxacin, clarithromycin, diclofenac, erythromycin, furosemide, ibuprofen, ketoprofen, naproxen, sulfamethoxazole, tetracycline, and triclosan were quantifiable in fish and shrimp samples.

Keywords: fish, liquid chromatography, mass spectrometry, pharmaceuticals, shrimp, solid-phase extraction

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Authors: Muslim Khan, Kenneth B. Jensen, Kevin A. Francesconi

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Trace amounts (ca 1 µg/L, 13 nM) of arsenic are present in sea water mostly as the oxyanion arsenate. In contrast, arsenic is present in marine biota (animals and algae) at very high levels (up to100,000 µg/kg) a significant portion of which is present as lipid-soluble compounds collectively termed arsenolipids. The complex nature of sea water presents an analytical challenge to detect trace compounds and monitor their environmental path. We developed a simple method using liquid-liquid extraction combined with HPLC-High Resolution Mass Spectrometer capable of detecting trace of arsenolipids (99 % of the sample matrix while recovering > 80 % of the six target arsenolipids with limit of detection of 0.003 µg/L.)

Keywords: arsenolipids, sea water, HPLC-high resolution mass spectrometry

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Authors: K. Jarmkom, P. Eakwaropas, W. Khobjai, S. Techaeoi

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Ancient Thai perfumed powder was used as a fragrance for clothing, food, and the body. Plant-based natural Thai perfume products are known as Pang-Rum. The objective of this study was to evaluate the stability of essential oils after six months of incubation. The chemical compositions were determined by gas chromatography-mass spectrometry (GC-MS), in terms of the qualitative composition of the isolated essential oil. The isolation of the essential oil of natural products by incubate sample for 5 min at 40 ºC is described. The volatile components were identified by percentage of total peak areas comparing their retention times of GC chromatograph with NIST mass spectral library. The results show no significant difference in the seven chromatograms of perfumed powder (Pang-Rum) both with binder and without binder. Further identification was done by GC-MS. Some components of Pang-Rum with/without binder were changed by temperature and time.

Keywords: GC-MS analysis, essential oils, stability, Pang-Rum

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Authors: Xavier A. Conlan

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Speed of analysis is a significant limitation to current high-performance liquid chromatography/mass spectrometry (HPLC/MS) and ultra-high-pressure liquid chromatography (UHPLC)/MS systems both of which are used in many forensic investigations. The flow rate limitations of MS detection require a compromise in the chromatographic flow rate, which in turn reduces throughput, and when using modern columns, a reduction in separation efficiency. Commonly, this restriction is combated through the post-column splitting of flow prior to entry into the mass spectrometer. However, this results in a loss of sensitivity and a loss in efficiency due to the post-extra column dead volume. A new chromatographic column format known as 'parallel segmented flow' involves the splitting of eluent flow within the column outlet end fitting, and in this study we present its application in order to interrogate the provenience of methamphetamine samples with mass spectrometry detection. Using parallel segmented flow, column flow rates as high as 3 mL/min were employed in the analysis of amino acids without post-column splitting to the mass spectrometer. Furthermore, when parallel segmented flow chromatography columns were employed, the sensitivity was more than twice that of conventional systems with post-column splitting when the same volume of mobile phase was passed through the detector. These finding suggest that this type of column technology will particularly enhance the capabilities of modern LC/MS enabling both high-throughput and sensitive mass spectral detection.

Keywords: chromatography, mass spectrometry methamphetamine, parallel segmented outlet flow column, forensic sciences

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Authors: Ramandeep Kaur, Ashok Kumar Malik

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Fabric Phase Sorptive Extraction (FPSE) combined with Gas chromatography Mass Spectrometry (GCMS) has been developed for the determination of nineteen organochlorine pesticides in various aqueous samples. The method consolidates the features of sol-gel derived microextraction sorbents with rich surface chemistry of cellulose fabric substrate which could directly extract sample from complex sample matrices and incredibly improve the operation with decreased pretreatment time. Some vital parameters such as kind and volume of extraction solvent and extraction time were examinedand optimized. Calibration curves were obtained in the concentration range 0.5-500 ng/mL. Under the optimum conditions, the limits of detection (LODs) were in the range 0.033 ng/mL to 0.136 ng/mL. The relative standard deviations (RSDs) for extraction of 10 ng/mL 0f OCPs were less than 10%. The developed method has been applied for the quantification of these compounds in aqueous and fruit juice samples. The results obtained proved the present method to be rapid and feasible for the determination of organochlorine pesticides in aqueous samples.

Keywords: fabric phase sorptive extraction, gas chromatography-mass spectrometry, organochlorine pesticides, sample pretreatment

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Authors: Mojtaba Heydarizad, Hamid Ghalibaf Mohammadabadi

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Iran is a semi-arid and arid country in south-western Asia in the Middle East facing intense climatological drought from the early times. Therefore, studying the precipitation events and the moisture sources and air masses causing precipitation has great importance in this region. In this study, the moisture sources and stable isotope content of precipitation moisture in three main events in 2015 have been studied in North-Eastern Iran. HYSPLIT model backward trajectories showed that the Caspian Sea and the mixture of the Caspian and Mediterranean Seas are dominant moisture sources for the studied events. This showed the role of cP (Siberian) and Mediterranean (MedT) air masses. Stable isotope studies showed that precipitation events originated from the Caspian Sea with lower Sea Surface Temperature (SST) have more depleted isotope values. However, precipitation events sourced from the mixture of the Caspian and the Mediterranean Seas (with higher SST) showed more enriched isotope values.

Keywords: HYSPLIT, Iran, Northern Khorasan, stable isotopes

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Authors: Ahmed M. Hjazi, Bader M. Hjazi

Abstract:

Protein 4.1 is a crucial component of complex interactions between the cytoskeleton and other junctional complex proteins. When the gene encoding this protein is altered, resulting in reduced expression, or when the protein is absent, the red cell undergoes a significant structural change. This research aims to achieve a deeper comprehension of the biochemical effects of red cell protein deficiency. A Tandem Mass Spectrometry Analysis (TMT-MS/MS) of patient cells lacking protein 4.1 compared to three healthy controls was achieved by the Proteomics Institute of the University of Bristol. The SDS-PAGE and Western blotting were utilized on the original patient sample and controls to partially confirm TMT MS/MS data analysis of the protein-4.1-deficient cells. Compared to healthy controls, protein levels in samples lacking protein 4.1 had a significantly higher concentration of proteins that probably originated from reticulocytes. This could occur if the patient has an elevated reticulocyte count. The increase in chaperone and reticulocyte-associated proteins was most notable in this study. This may result from elevated quantities of reticulocytes in patients with hereditary elliptocytosis.

Keywords: hereditary elliptocytosis, protein 4.1, red cells, tandem mass spectrometry data.

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Authors: Belhaj Mohamed, M. Saidi, I. Bouazizi, M. Soussi, M. Ben Jrad

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The Late Cenomanian-Early Turonian laminated, black, organic-rich limestones were described in Central Tunisia and attributed to the Bahloul Formation. It covers central and northern Tunisia, and the northern part of the Gulf of Gabes. The Bahloul Formation is considered as one of the main source rocks in Tunisia and is composed of outer-shelf to slop-laminated and dark-gray to black-colored limestones and marls. This formation had been deposited in a relatively deep-marine, calm, and anoxic environment. Rock-Eval analysis and vitrinite reflectance (Ro) measurements were performed on the basis of the organic carbon content. Several samples were chosen for molecular organic geochemistry. Saturate and aromatic hydrocarbons were analyzed by gas chromatography (GC) and GC–mass spectrometry. Geochemical data of the Bahloul Formation in northern and central Tunisia show this level to be a good potential source rock as indicated by the high content of type II organic matter. This formation exhibits high total organic carbon contents (as much as 14%), with an average value of 2% and a good to excellent petroleum potential, ranging between 2 and 50 kg of hydrocarbon/ton of rock. The extracts from the Bahloul Formation are characterized by Pr/Ph ratios ranging between 1.5 and 3, a moderate diasterane content, a C27 sterane approximately equal to C29 sterane, a high C28/C29 ratio, low gammacerane index, a C35/C34 homohopane ratio less than 1 and carbon isotope compositions between -24 and -26‰. The thermal maturity is relatively low, corresponding to the beginning of the oil window in the western area near the Algerian border, in the oil window in the eastern area (Sahel basin) and late mature in northern part.

Keywords: biomarkers, organic geochemistry, source rock, Tunisia

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Authors: Godwin Dennison, C. E. Boulind, O. Gould, B. de Lacy Costello, J. Allison, P. White, P. Ewings, A. Wicaksono, N. J. Curtis, A. Pullyblank, D. Jayne, J. A. Covington, N. Ratcliffe, N. K. Francis

Abstract:

Background: Colorectal symptoms are common but only infrequently represent serious pathology, including colorectal cancer (CRC). A large number of invasive tests are presently performed for reassurance. We investigated the feasibility of urinary volatile organic compound (VOC) testing as a potential triage tool in patients fast-tracked for assessment for possible CRC. Methods: A prospective, multi-centre, observational feasibility study was performed across three sites. Patients referred on NHS fast-track pathways for potential CRC provided a urine sample which underwent Gas Chromatography Mass Spectrometry (GC-MS), Field Asymmetric Ion Mobility Spectrometry (FAIMS) and Selected Ion Flow Tube Mass Spectrometry (SIFT-MS) analysis. Patients underwent colonoscopy and/or CT colonography and were grouped as either CRC, adenomatous polyp(s), or controls to explore the diagnostic accuracy of VOC output data supported by an artificial neural network (ANN) model. Results: 558 patients participated with 23 (4.1%) CRC diagnosed. 59% of colonoscopies and 86% of CT colonographies showed no abnormalities. Urinary VOC testing was feasible, acceptable to patients, and applicable within the clinical fast track pathway. GC-MS showed the highest clinical utility for CRC and polyp detection vs. controls (sensitivity=0.878, specificity=0.882, AUROC=0.884). Conclusion: Urinary VOC testing and analysis are feasible within NHS fast-track CRC pathways. Clinically meaningful differences between patients with cancer, polyps, or no pathology were identified therefore suggesting VOC analysis may have future utility as a triage tool. Acknowledgment: Funding: NIHR Research for Patient Benefit grant (ref: PB-PG-0416-20022).

Keywords: colorectal cancer, volatile organic compound, gas chromatography mass spectrometry, field asymmetric ion mobility spectrometry, selected ion flow tube mass spectrometry

Procedia PDF Downloads 55

Authors: Long Wang, Yongjin Feng, Xiaofang Luo

Abstract:

Tritium permeation through structural materials is a significant issue for fusion demonstration (DEMO) reactor blankets in terms of fuel cycle efficiency and radiological safety. Reduced activation ferritic (RAFM) steel CLF-1 is a prime candidate for the China’s CFETR blanket structural material, facing high permeability of hydrogen isotopes at reactor operational temperature. To confine tritium as much as possible in the reactor, surface modification of the steels including fabrication of tritium permeation barrier (TPB) attracts much attention. As a new alloy system, high entropy alloy (HEA) contains at least five principal elements, each of which ranges from 5 at% to 35 at%. This high mixing effect entitles HEA extraordinary comprehensive performance. So it is attractive to lead HEA into surface alloying for protective use. At present, studies on the hydrogen isotope permeability of HEA coatings is still insufficient and corresponding mechanism isn’t clear. In our study, we prepared three kinds of HEA coatings, including AlCrTaTiZr, (AlCrTaTiZr)N and (AlCrTaTiZr)O. After comprehensive characterization of SEM, XPS, AFM, XRD and TEM, the structure and composition of the HEA coatings were obtained. Deuterium permeation tests were conducted to evaluate the hydrogen isotope permeability of AlCrTaTiZr, (AlCrTaTiZr)N and (AlCrTaTiZr)O HEA coatings. Results proved that the (AlCrTaTiZr)N and (AlCrTaTiZr)O HEA coatings had better hydrogen isotope permeation resistance. Through analyzing and characterizing the hydrogen isotope permeation results of the corroded samples, an internal link between hydrogen isotope permeation behavior and structure of HEA coatings was established. The results provide valuable reference in engineering design of structural and TPB materials for future fusion device.

Keywords: high entropy alloy, hydrogen isotope permeability, tritium permeation barrier, fusion demonstration reactor

Procedia PDF Downloads 142

Authors: Ece Kök Yetimoğlu, Soner Çubuk, Neşe Taşci, M. Vezir Kahraman

Abstract:

Lead(II) is one of the most toxic environmental pollutants in the world, due to its high toxicity and non-biodegradability. Lead exposure causes severe risks to human health such as central brain damages, convulsions, kidney damages, and even death. To determine lead(II) in environmental or biological samples, scientists use atomic absorption spectrometry (AAS), inductively coupled plasma mass spectrometry (ICPMS), fluorescence spectrometry and electrochemical techniques. Among these systems the fluorescence spectrometry and fluorescent chemical sensors have attracted considerable attention because of their good selectivity and high sensitivity. The fluorescent polymers usually contain covalently bonded fluorophores. In this study imidazole based UV cured polymeric film was prepared and designed to act as a fluorescence chemo sensor for lead (II) analysis. The optimum conditions such as influence of pH value and time on the fluorescence intensity of the sensor have also been investigated. The sensor was highly sensitive with a detection limit as low as 1.87 × 10−8 mol L-1 and it was successful in the determination of Pb(II) in water samples.

Keywords: fluorescence, lead(II), photopolymerization, polymeric sensor

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