Search results for: gas chromatography mass spectrometer

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: Tengku Muhammad Rafi Nazmi Bin Tengku Razali, Habsah Alwi

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This article based on effect of temperature towards extraction of Aquilaria Subintegra. Aquilaria Subintegra which its main habitat is in Asia-tropical and particularly often found in its native which is Thailand. There is claim which is Aquilaria Subintegra contains antipyretic properties that helps fight fever. Research nowadays also shown that paracetamol consumed bring bad effect towards consumers. This sample will first dry using Vacuum Far Infrared which provides better drying than conventional oven. Soxhlet extractor used to extract oil from sample. Gas Chromatography Mass Spectrometer used to analyze sample to determine its compound. Objective from this research was to determine the active ingredients that exist in the Aquilaria Subintegra leaves and to determine whether compound of Acetaminophen exist or not inside the leaves. Moisture content from 400C was 80%, 500C was 620% and 600C was 36%. The greater temperature resulting lower moisture content inside sample leaves. 7 components were identified in sample T=400C while only 5 components were identified in sample at T=50C and T=60C. Four components were commonly identified in three sample which is 1n-Hexadecanoic acid, 9,12,15-Octadecatrienoic acid, methyl ester (z,z,z), Vitamin E and Squalene. Further studies are needed with new series of temperature to refine the best results.

Keywords: aquilaria subintegra, vacuum far infrared, SOXHLET extractor, gas chromatography mass spectrometer, paracetamol

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Authors: Rowan Moore, Kai Scheffler, Eugen Damoc, Jennifer Sutton, Aaron Bailey, Stephane Houel, Simon Cubbon, Jonathan Josephs

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Purpose: MS analysis of monoclonal antibodies (mAbs) at the protein and peptide levels is critical during development and production of biopharmaceuticals. The compositions of current generation therapeutic proteins are often complex due to various modifications which may affect efficacy. Intact proteins analyzed by MS are detected in higher charge states that also provide more complexity in mass spectra. Protein analysis in native or native-like conditions with zero or minimal organic solvent and neutral or weakly acidic pH decreases charge state value resulting in mAb detection at higher m/z ranges with more spatial resolution. Methods: Three commercially available mAbs were used for all experiments. Intact proteins were desalted online using size exclusion chromatography (SEC) or reversed phase chromatography coupled on-line with a mass spectrometer. For streamlined use of the LC- MS platform we used a single SEC column and alternately selected specific mobile phases to perform separations in either denaturing or native-like conditions: buffer A (20 % ACN, 0.1 % FA) with Buffer B (100 mM ammonium acetate). For peptide analysis mAbs were proteolytically digested with and without prior reduction and alkylation. The mass spectrometer used for all experiments was a commercially available Thermo Scientific™ hybrid Quadrupole-Orbitrap™ mass spectrometer, equipped with the new BioPharma option which includes a new High Mass Range (HMR) mode that allows for improved high mass transmission and mass detection up to 8000 m/z. Results: We have analyzed the profiles of three mAbs under reducing and native conditions by direct infusion with offline desalting and with on-line desalting via size exclusion and reversed phase type columns. The presence of high salt under denaturing conditions was found to influence the observed charge state envelope and impact mass accuracy after spectral deconvolution. The significantly lower charge states observed under native conditions improves the spatial resolution of protein signals and has significant benefits for the analysis of antibody mixtures, e.g. lysine variants, degradants or sequence variants. This type of analysis requires the detection of masses beyond the standard mass range ranging up to 6000 m/z requiring the extended capabilities available in the new HMR mode. We have compared each antibody sample that was analyzed individually with mixtures in various relative concentrations. For this type of analysis, we observed that apparent native structures persist and ESI is benefited by the addition of low amounts of acetonitrile and formic acid in combination with the ammonium acetate-buffered mobile phase. For analyses on the peptide level we analyzed reduced/alkylated, and non-reduced proteolytic digests of the individual antibodies separated via reversed phase chromatography aiming to retrieve as much information as possible regarding sequence coverage, disulfide bridges, post-translational modifications such as various glycans, sequence variants, and their relative quantification. All data acquired were submitted to a single software package for analysis aiming to obtain a complete picture of the molecules analyzed. Here we demonstrate the capabilities of the mass spectrometer to fully characterize homogeneous and heterogeneous therapeutic proteins on one single platform. Conclusion: Full characterization of heterogeneous intact protein mixtures by improved mass separation on a quadrupole-Orbitrap™ mass spectrometer with extended capabilities has been demonstrated.

Keywords: disulfide bond analysis, intact analysis, native analysis, mass spectrometry, monoclonal antibodies, peptide mapping, post-translational modifications, sequence variants, size exclusion chromatography, therapeutic protein analysis, UHPLC

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Authors: A. B. Bazaralieva, A. A. Turgumbayeva

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: Allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Bazaraliyeva Aigerim Bakytzhanovna, Turgumbayeva Aknur Amanbekovna

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Cristian Moisa, Andreea Lupitu, Adriana Csakvari, Dana G. Radu, Leonard Marian Olariu, Georgeta Pop, Dorina Chambre, Lucian Copolovici, Dana Copolovici

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Green synthesis of nanoparticles (NPs) represents a promising, accessible, eco-friendly, and safe process with significant applications in biotechnology, pharmaceutical sciences, and farming. The aim of our study was to obtain silver nanoparticles, using plant wastes extracts resulted in the essential oils extraction process: Thymus vulgaris L., Origanum vulgare L., Lavandula angustifolia L., and in hemp processing for seed and fibre, Cannabis sativa. Firstly, we obtained aqueous extracts of thyme, oregano, lavender, and hemp (two monoicous and one dioicous varieties), all harvested in western part of Romania. Then, we determined the chemical composition of the extracts by liquid-chromatography coupled with diode array and mass spectrometer detectors. The compounds identified in the extracts were in agreement with earlier published data, and the determination of the antioxidant activity of the obtained extracts by DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)) assays confirmed their antioxidant activity due to their total polyphenolic content evaluated by Folin-Ciocalteu assay. Then, the silver nanoparticles (AgNPs) were successfully biosynthesised, as was demonstrated by UV-VIS, FT-IR spectroscopies, and SEM, by reacting AgNO₃ solution and plant extracts. AgNPs were spherical in shape, with less than 30 nm in diameter, and had a good bactericidal activity against Gram-positive (Staphylococcus aureus) and Gram-negative bacteria (Escherichia coli, Klebsiella pneumoniae, Pseudomonas fluorescens).

Keywords: plant wastes extracts, chemical composition, high performance liquid chromatography mass spectrometer, HPLC-MS, scanning electron microscopy, SEM, silver nanoparticles

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Authors: Béla Kovács, Éva Bódi, Farzaneh Garousi, Szilvia Várallyay, Dávid Andrási

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For analysis of elements in different food, feed and food raw material samples generally a flame atomic absorption spectrometer (FAAS), a graphite furnace atomic absorption spectrometer (GF-AAS), an inductively coupled plasma optical emission spectrometer (ICP-OES) and an inductively coupled plasma mass spectrometer (ICP-MS) are applied. All the analytical instruments have different physical and chemical interfering effects analysing food and food raw material samples. The smaller the concentration of an analyte and the larger the concentration of the matrix the larger the interfering effects. Nowadays, it is very important to analyse growingly smaller concentrations of elements. From the above analytical instruments generally the inductively coupled plasma mass spectrometer is capable of analysing the smallest concentration of elements. The applied ICP-MS instrument has Collision Cell Technology (CCT) also. Using CCT mode certain elements have better detection limits with 1-3 magnitudes comparing to a normal ICP-MS analytical method. The CCT mode has better detection limits mainly for analysis of selenium (arsenic, germanium, vanadium, and chromium). To elaborate an analytical method for selenium with an inductively coupled plasma mass spectrometer the most important interfering effects (problems) were evaluated: 1) isobaric elemental, 2) isobaric molecular, and 3) physical interferences. Analysing food and food raw material samples an other (new) interfering effect emerged in ICP-MS, namely the effect of various matrixes having different evaporation and nebulization effectiveness, moreover having different quantity of carbon content of food, feed and food raw material samples. In our research work the effect of different water-soluble compounds furthermore the effect of various quantity of carbon content (as sample matrix) were examined on changes of intensity of selenium. So finally we could find “opportunities” to decrease the error of selenium analysis. To analyse selenium in food, feed and food raw material samples, the most appropriate inductively coupled plasma mass spectrometer is a quadrupole instrument applying a collision cell technique (CCT). The extent of interfering effect of carbon content depends on the type of compounds. The carbon content significantly affects the measured concentration (intensities) of Se, which can be corrected using internal standard (arsenic or tellurium).

Keywords: selenium, ICP-MS, food, food raw material

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Authors: Jun Yang, Norbert Schulz, Claude Canizares

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Knowing the dust content in the interstellar matter is necessary to understand the composition and evolution of the interstellar medium (ISM). The metal composition of the ISM enables us to study the cooling and heating processes that dominate the star formation rates in our Galaxy. The Chandra High Energy Transmission Grating (HETG) Spectrometer provides a unique opportunity to measure element dust compositions through X-ray edge absorption structure. We measure gas to dust optical depth ratios towards 9 bright Low-Mass X-ray Binaries (LMXBs) in the Galactic Bulge with the highest precision so far. Well calibrated and pile-up free optical depths are measured with the HETG spectrometer with respect to broadband hydrogen equivalent absorption in bright LMXBs: 4U 1636-53, Ser X-1, GX 3+1, 4U 1728-34, 4U 1705-44, GX 340+0, GX 13+1, GX 5-1, and GX 349+2. From the optical depths results, we deduce gas to dust ratios for various silicates in the ISM and present our results for the Si K edge in different lines of sight towards the Galactic Bulge.

Keywords: low-mass X-ray binaries, interstellar medium, gas to dust ratio, spectrometer

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Authors: Nabil Jallouli, Luisa M. Pastrana-Martínez, Ana R. Ribeiro, Nuno F. F. Moreira, Joaquim L. Faria, Olfa Hentati, Adrián M. T. Silva, Mohamed Ksibi

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Degradation and mineralization of ibuprofen (IBU) were investigated using Ultraviolet (UV) Light Emitting Diodes (LEDs) in TiO2 photocatalysis. Samples of ultrapure water (UP) and a secondary treated effluent of a municipal wastewater treatment plant (WWTP), both spiked with IBU, as well as a highly concentrated IBU (230 mgL-1) pharmaceutical industry wastewater (PIWW), were tested in the TiO2/UV-LED system. Three operating parameters, namely, pH, catalyst load and number of LEDs were optimized. The process efficiency was evaluated in terms of IBU removal using high performance liquid chromatography (HPLC) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Additionally, the mineralization was investigated by determining the dissolved organic carbon (DOC) content. The chemical structures of transformation products were proposed based on the data obtained using liquid chromatography with a high resolution mass spectrometer ion trap/time-of-flight (LC-MS-IT-TOF). A possible pathway of IBU degradation was accordingly proposed. Bioassays were performed using the marine bacterium Vibrio fischeri to evaluate the potential acute toxicity of original and treated wastewaters. TiO2 heterogeneous photocatalysis was efficient to remove IBU from UP and from PIWW, and less efficient in treating the wastewater from the municipal WWTP. The acute toxicity decreased by ca. 40% after treatment, regardless of the studied matrix.

Keywords: acute toxicity, Ibuprofen, UV-LEDs, wastewaters

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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: 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: Nadeem A. Siddique, Mohd Mujeeb, Kahkashan

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Introduction: The objective of the projected work is to study the occurrence of the aflatoxins B1, B2, G1and G2 in remedial plants, exclusively in Delphinium denudatum. The aflatoxins were analysed by high-performance liquid chromatography–tandem quadrupole mass spectrometry with electrospray ionization (HPLC–MS/MS) and immunoaffinity column chromatography were used for extraction and purification of aflatoxins. PDA media was selected for fungal count. Results: A good quality linear relationship was originated for AFB1, AFB2, AFG1 and AFG2 at 1–10 ppb (r > 0.9995). The analyte precision at three different spiking levels was 88.7–109.1 %, by means of low per cent relative standard deviations in each case. Within 5 to7 min aflatoxins can be separated using an Agilent XDB C18-column. We found that AFB1 and AFB2 were not found in D. denudatum. This was reliable through exceptionally low figures of fungal colonies observed after 6 hr of incubation. The developed analytical method is straightforward, be successfully used to determine the aflatoxins. Conclusion: The developed analytical method is straightforward, simple, accurate, economical and can be successfully used to find out the aflatoxins in remedial plants and consequently to have power over the quality of products. The presence of aflatoxin in the plant extracts was interrelated to the least fungal load in the remedial plants examined.

Keywords: aflatoxins, delphinium denudatum, liquid chromatography, mass spectrometry

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Authors: Moses C. Siame, Kazutoshi Haga, Atsushi Shibayama

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This study investigates the removal of silica, alumina and phosphorus as impurities from Sanje iron ore using wet high-intensity magnetic separation (WHIMS). Sanje iron ore contains low-grade hematite ore found in Nampundwe area of Zambia from which iron is to be used as the feed in the steelmaking process. The chemical composition analysis using X-ray Florence spectrometer showed that Sanje low-grade ore contains 48.90 mass% of hematite (Fe₂O₃) with 34.18 mass% as an iron grade. The ore also contains silica (SiO₂) and alumina (Al₂O₃) of 31.10 mass% and 7.65 mass% respectively. The mineralogical analysis using X-ray diffraction spectrometer showed hematite and silica as the major mineral components of the ore while magnetite and alumina exist as minor mineral components. Mineral particle distribution analysis was done using scanning electron microscope with an X-ray energy dispersion spectrometry (SEM-EDS) and images showed that the average mineral size distribution of alumina-silicate gangue particles is in order of 100 μm and exists as iron-bearing interlocked particles. Magnetic separation was done using series L model 4 Magnetic Separator. The effect of various magnetic separation parameters such as magnetic flux density, particle size, and pulp density of the feed was studied during magnetic separation experiments. The ore with average particle size of 25 µm and pulp density of 2.5% was concentrated using pulp flow of 7 L/min. The results showed that 10 T was optimal magnetic flux density which enhanced the recovery of 93.08% of iron with 53.22 mass% grade. The gangue mineral particles containing 12 mass% silica and 3.94 mass% alumna remained in the concentrate, therefore the concentrate was further treated in the second stage WHIMS using the same parameters from the first stage. The second stage process recovered 83.41% of iron with 67.07 mass% grade. Silica was reduced to 2.14 mass% and alumina to 1.30 mass%. Accordingly, phosphorus was also reduced to 0.02 mass%. Therefore, the two stage magnetic separation process was established using these results.

Keywords: Sanje iron ore, magnetic separation, silica, alumina, recovery

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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: R. Mickiene, A. Friese, U. Rosler, A. Maruska, O. Ragazinskiene

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This research focuses on phytochemistry and antimicrobial activities of compounds isolated and identified from three species of Eryngium. The antimicrobial activity of extracts from Eryngiumplanum L., Eryngium maritimum L., Eryngium campestre L. grown in Lithuania, were tested by the method of series dilutions, against different bacteria species: Escherichia coli, Proteus vulgaris and Staphylococcus aureus with and without antibiotic resistances, originating from livestock. The antimicrobial activity of extracts was described by determination of the minimal inhibitory concentration. Preliminary results show that the minimal inhibitory concentration range between 8.0 % and 17.0 % for the different Eryngium extracts and bacterial species.The total amounts ofphenolic compounds and total amounts of flavonoids were tested in the methanolic extracts of the plants. Identification and evaluation of the phenolic compounds were performed by liquid chromatography. The essential oils were analyzed by gas chromatography mass spectrometry.

Keywords: antimicrobial activities, Eryngium L. species, essential oils, gas chromatography mass spectrometry

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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: Methaq Algabr, Nabil Al-Hajj, Ameerh Jaber, Amtellah Alshotobi, Shaima'a Al-suryhi, Gadah Whaban, Nawal Alshehari

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Steam distillation of the essential oil of P. jaubertii was performed using a Clevenger apparatus. Essential oils were analyzed by gas chromatography-flame ionization detector (GC-FID) and gas chromatography coupled to chromatography–mass spectrometry (GC-MS). The major chemical components identified in P. jaubertii essential oil include carvotanacetone (63.975%), 1-methyl-1,2-propanedione (5.887%), 2,5-dimethoxy-para-cymene (3.303%) and ar-curcumene (3.276%). The antimicrobial activity of the essential oil of P. jaubertii was evaluated against all tested microorganisms. P. jaubertii essential oil inhibited all tested microorganisms except Escherichia coli with a minimum inhibitory concentration (MIC) of 5.0 μg/mL against Staphylococcus aureus.

Keywords: Pulicaria jaubertii, essential oil, antimicrobial, Carvotancetone

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Authors: Jijun Shi, Lichen Sun, Jianchao Zhao, Lizhi Sun, Enjun Liu, Chongwu Guo

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Because of the consistency of pressure direction, more short cycle, and high sensitivity, Charging-Vacuum helium mass spectrometer leak testing technology is the most popular leak testing technology for the seal testing of the spacecraft parts, especially the small and medium size ones. Usually, auxiliary pump was used, and the minimum detectable leak rate could reach 5E-9Pa•m3/s, even better on certain occasions. Relative error is more important when evaluating the results. How to choose the reference leak, the background level of helium, and record formats would affect the leak rate tested. In the linearity range of leak testing system, it would reduce 10% relative error if the reference leak with larger leak rate was used, and the relative error would reduce obviously if the background of helium was low efficiently, the record format of decimal was used, and the more stable data were recorded.

Keywords: leak testing, spacecraft parts, relative error, error control

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Authors: Bernadett Henn, Katalin Tálos, Éva Kováss Széles

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During the last 50 years, the worldwide permeation of the nuclear techniques induces several new problems in the environmental and in the human life. Nowadays, due to the increasing of the risk of terrorism worldwide, the potential occurrence of terrorist attacks using also weapon of mass destruction containing radioactive or nuclear materials as e.g. dirty bombs, is a real threat. For instance, the uranium pellets are one of the potential nuclear materials which are suitable for making special weapons. The nuclear forensics mainly focuses on the determination of the origin of the confiscated or found nuclear and other radioactive materials, which could be used for making any radioactive dispersive device. One of the most important signatures in nuclear forensics to find the origin of the material is the determination of the rare earth element patterns (REE) in the seized or found radioactive or nuclear samples. The concentration and the normalized pattern of the REE can be used as an evidence of uranium origin. The REE are the fourteen Lanthanides in addition scandium and yttrium what are mostly found together and really low concentration in uranium pellets. The problems of the REE determination using ICP-MS technique are the uranium matrix (high concentration of uranium) and the interferences among Lanthanides. In this work, our aim was to develop an effective chemical sample preparation process using extraction chromatography for separation the uranium matrix and the rare earth elements from each other following some publications can be found in the literature and modified them. Secondly, our purpose was the optimization of the ICP-MS measuring process for REE concentration. During method development, in the first step, a REE model solution was used in two different types of extraction chromatographic resins (LN® and TRU®) and different acidic media for environmental testing the Lanthanides separation. Uranium matrix was added to the model solution and was proved in the same conditions. Methods were tested and validated using REE UOC (uranium ore concentrate) reference materials. Samples were analyzed by sector field mass spectrometer (ICP-SFMS).

Keywords: extraction chromatography, nuclear forensics, rare earth elements, uranium

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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: 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: Athena Nguyen, Rojin Belganeh

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Detecting and identifying differences in like polymer materials are key factors in deformulation, comparative analysis as well as 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. This presentation demonstrates the study of two similar polymers by performing different mode of operations in the same system: Evolve gas analysis (EGA), Flash pyrolysis, Thermal desorption analysis, and Heart-cutting analysis. Unknown polymer materials and their chemical compositions are identified.

Keywords: gas chromatography/mass spectrometry, pyrolysis, pyrolyzer, thermal desorption-GC/MS

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Authors: Fangyan Li, Lin Min Lee, Hui Zhu Peh, Shoet Harn Chan

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Advantame, a derivative of aspartame, is the latest addition to a family of low caloric and high potent dipeptide sweeteners which include aspartame, neotame and alitame. The use of advantame as a high-intensity sweetener in food was first accepted by Food Standards Australia New Zealand in 2011 and subsequently by US and EU food authorities in 2014, with the results from toxicity and exposure studies showing advantame poses no safety concern to the public at regulated levels. To our knowledge, currently there is barely any detailed information on the analytical method of advantame in food matrix, except for one report published in Japanese, stating a high performance liquid chromatography (HPLC) and liquid chromatography/ mass spectrometry (LC-MS) method with a detection limit at ppm level. However, the use of acid in sample preparation and instrumental analysis in the report raised doubt over the reliability of the method, as there is indication that stability of advantame is compromised under acidic conditions. Besides, the method may not be suitable for analyzing food matrices containing advantame at low ppm or sub-ppm level. In this presentation, a simple, specific and sensitive method for the determination of advantame in food is described. The method involved extraction with water and clean-up via solid phase extraction (SPE) followed by detection using liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative electrospray ionization mode. No acid was used in the entire procedure. Single laboratory validation of the method was performed in terms of linearity, precision and accuracy. A low detection limit at ppb level was achieved. Satisfactory recoveries were obtained using spiked samples at three different concentration levels. This validated method could be used in the routine inspection of the advantame level in food.

Keywords: advantame, food, LC-MS/MS, sweetener

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Authors: G. Ozturk, B. Demirci

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It is well known that essential oils used for therapeutic purposes for many years. In this study, five different Pharmacopoeia grade essential oils (Achillea millefolium L., Pimpinella anisum L., Matricaria recutita L., Eucalyptus globulus L., Salvia officinalis L.) which obtained from commercial sources were evaluated for chemical compositions, synergistic antimicrobial activities, and lipoxygenase enzyme inhibitions. Volatile components were determined by gas chromatography/flame ionization detector and gas chromatography/mass spectrometer, simultaneously. The potential antimicrobial activity of essential oils was tested against oral pathogenic standard strains such as Streptococcus mutans, Streptococcus sanguinis, Staphylococcus aureus, Corynebacterium striatum, Candida albicans and Candida krusei by broth microdilution methods. Ciprofloxacin and ketoconazole were used positive controls. It has been observed that the essential oils tested have average inhibitory antimicrobial activity against oral pathogens with a Minimum Inhibition Concentration of 20-0.625 mg/mL. The active essential oils have been combined with antibiotics and synergistic effects have been evaluated by Checkerboard method. ƩFIC values were determined. In combination with antibiotics M. recutita essential oil has been shown to have a synergistic effect against S. aureus in combination with tetracycline (ƩFIC 0.46). In addition, 5-LOX inhibitory activity was measured by modifying the spectrophotometric method developed by Baylac and Racine. As a result, 5-LOX % inhibition of S. officinalis, E. globulus and M. recutita were calculated as 34.0 ± 6.66, 72.7 ± 2.78 and 27.7 ± 0.60, respectively.

Keywords: antimicrobial activity, essential oils, synergistic activity, 5-lipoxygenase inhibition

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Authors: Béla Kovács, Éva Bódi, Farzaneh Garousi, Szilvia Várallyay, Áron Soós, Xénia Vágó, Dávid Andrási

Abstract:

In agriculture for analysis of elements in different food and food raw materials, moreover environmental samples generally flame atomic absorption spectrometers (FAAS), graphite furnace atomic absorption spectrometers (GF-AAS), inductively coupled plasma optical emission spectrometers (ICP-OES) and inductively coupled plasma mass spectrometers (ICP-MS) are routinely applied. An inductively coupled plasma mass spectrometer (ICP-MS) is capable for analysis of 70-80 elements in multielemental mode, from 1-5 cm3 volume of a sample, moreover the detection limits of elements are in µg/kg-ng/kg (ppb-ppt) concentration range. All the analytical instruments have different physical and chemical interfering effects analysing the above types of samples. The smaller the concentration of an analyte and the larger the concentration of the matrix the larger the interfering effects. Nowadays there is very important to analyse growingly smaller concentrations of elements. From the above analytical instruments generally the inductively coupled plasma mass spectrometer is capable of analysing the smallest concentration of elements. The applied ICP-MS instrument has Collision Cell Technology (CCT) also. Using CCT mode certain elements have better (smaller) detection limits with 1-3 magnitudes comparing to a normal ICP-MS analytical method. The CCT mode has better detection limits mainly for analysis of selenium, arsenic, germanium, vanadium and chromium. To elaborate an analytical method for trace elements with an inductively coupled plasma mass spectrometer the most important interfering effects (problems) were evaluated: 1) Physical interferences; 2) Spectral interferences (elemental and molecular isobaric); 3) Effect of easily ionisable elements; 4) Memory interferences. Analysing food and food raw materials, moreover environmental samples an other (new) interfering effect emerged in ICP-MS, namely the effect of various matrixes having different evaporation and nebulization effectiveness, moreover having different quantity of carbon content of food and food raw materials, moreover environmental samples. In our research work the effect of different water-soluble compounds furthermore the effect of various quantity of carbon content (as sample matrix) were examined on changes of intensity of the applied elements. So finally we could find “opportunities” to decrease or eliminate the error of the analyses of applied elements (Cr, Co, Ni, Cu, Zn, Ge, As, Se, Mo, Cd, Sn, Sb, Te, Hg, Pb, Bi). To analyse these elements in the above samples, the most appropriate inductively coupled plasma mass spectrometer is a quadrupole instrument applying a collision cell technique (CCT). The extent of interfering effect of carbon content depends on the type of compounds. The carbon content significantly affects the measured concentration (intensities) of the above elements, which can be corrected using different internal standards.

Keywords: elements, environmental and food samples, ICP-MS, interference effects

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Authors: Xingyu Peng, Qingyuan Hu, Xuebin Zhu, Xi Yuan

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Neutron spectrometry has contributed much to the development of nuclear physics since 1932 and has also become an importance tool in several other fields, notably nuclear technology, fusion plasma diagnostics and radiation protection. Compared with neutron fluxes, neutron spectra can provide more detailed information on the internal physical process of neutron sources, such as fast neutron reactors, fusion plasma, fission-fusion hybrid reactors, and so on. However, high performance neutron spectrometer is not so commonly available as it requires the use of large and complex instrumentation. This work describes the development and characterization of a compact magnetic proton recoil (MPR) spectrometer for high-resolution measurements of fast neutron spectra. The compact MPR spectrometer is featured by its large recoil angle, small size permanent analysis magnet, short beam transport line and dual-purpose detector array for both steady state and pulsed neutron spectra measurement. A 3-dimensional electromagnetic particle transport code is developed to simulate the response function of the spectrometer. Simulation results illustrate that the performance of the spectrometer is mainly determined by n-p recoil foil and proton apertures, and an overall energy resolution of 3% is achieved for 14 MeV neutrons. Dedicated experiments using alpha source and mono-energetic neutron beam are employed to verify the simulated response function of the compact MPR spectrometer. These experimental results show a good agreement with the simulated ones, which indicates that the simulation code possesses good accuracy and reliability. The compact MPR spectrometer described in this work is a valuable tool for fast neutron spectra measurements for the fission or fusion devices.

Keywords: neutron spectrometry, magnetic proton recoil spectrometer, neutron spectra, fast neutron

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Authors: B. Bakchiche, H. Guenane, M. Bireche, A. Noureddinne, A. Gherib

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The chemical composition of the essential oils obtained by hydrodistillation from Artemisia campestris L (family Asteraceae) collected in Djebel Amour (Sahara Atlas, Algeria). Aerial parts were also evaluated by gas chromatography (GC) and gas chromatography coupled to mass spectrometry (GC-MS). The analyses for leaves and fruits of A. campestris resulted in the identification of thirty-one compounds, representing 91.8 % of the total oil and the yields were 0.33% (v/dry weight). The main components were β-pinene and sabinene (25.6% and 17% respectively) followed by α-pinene (9.9%), limonene (6.6 %) and p-cymene (4.1%).

Keywords: essential oil, GC-MS, Artemesia campestris, Algeria

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Authors: Bashar Al-Sabti, Jehad Harbali

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Background: Pyridine is a reactive base that might be used in preparing sitagliptin. International Agency for Research on Cancer classifies pyridine in group 2B; this classification means that pyridine is possibly carcinogenic to humans. Therefore, pyridine should be monitored at the allowed limit in sitagliptin pharmaceutical ingredients. Objective: The aim of this study was to develop a novel ultra high performance liquid chromatography mass spectrometry (UHPLC-MS) method to estimate the quantity of pyridine impurity in sitagliptin pharmaceutical ingredients. Methods: The separation was performed on C8 shim-pack (150 mm X 4.6 mm, 5 µm) in reversed phase mode using a mobile phase of water-methanol-acetonitrile containing 4 mM ammonium acetate in gradient mode. Pyridine was detected by mass spectrometer using selected ionization monitoring mode at m/z = 80. The flow rate of the method was 0.75 mL/min. Results: The method showed excellent sensitivity with a quantitation limit of 1.5 ppm of pyridine relative to sitagliptin. The linearity of the method was excellent at the range of 1.5-22.5 ppm with a correlation coefficient of 0.9996. Recoveries values were between 93.59-103.55%. Conclusions: The results showed good linearity, precision, accuracy, sensitivity, selectivity, and robustness. The studied method was applied to test three batches of sitagliptin raw materials. Highlights: This method is useful for monitoring pyridine in sitagliptin during its synthesis and testing sitagliptin raw materials before using them in the production of pharmaceutical products.

Keywords: genotoxic impurity, pyridine, sitagliptin, UHPLC -MS

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Authors: Min Sik Kim, Hwa Sung Shin

Abstract:

From 2013, small eel farms, which are located in Han River Estuary, South Korea suffer damage because of unknown massive perish. In the middle of discussion that the cause of perish could be environmental changes or waste water, a large amount of unknown nemertean was discovered during that time. Some nemerteans are known releasing neurotoxin substance. In this study, we isolated intestinal bacteria using selective media and conducted 16s rDNA microbial identification by gene alignment. As a result, there was a type of bacteria producing TTX, blocks sodium-channel inducing organism’s death. TTX production from the bacteria was confirmed by ELISA and liquid chromatography coupled with mass spectrometer. Additionally, the activated-charcoal which has an ability to absorb small molecules like toxin was applied to fibrous mesh to prevent ingestion of aquatic organisms and increase applicable area. The viability of zebrafish in the water with TTX and charcoal fiber mat were not decreased meaning it could be used for solving the perishing problem in fish farm.

Keywords: nemertean, TTX, fiber mat, activated charcoal, zebrafish

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

Abstract:

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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