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Optimalizace a validace metody stanovení volných mastných kyselin / The optimization and validation of the method for assessment of free fatty acidsSýkora, Michal January 2016 (has links)
This master thesis deals with the development of method for free fatty acids determination in natural and processed cheese. In the theoretical part the possibilities of extraction, fractionation and determination of lipid fractions, characterization of fatty acids and various methods of their determination are described, as well as determination of free fatty acids. The main scope of the experimental section is optimization and validation of the selected method for determination of free fatty acids in various cheese matrices. For extraction of lipids from the sample the method with the mixture of diethylether and petrolether according to ČSN EN ISO 1735 was selected. Thin-layer chromatography and solid phase extraction were tested and compared for separation of free fatty acids. The method according to ČSN EN ISO 5509, using methanol solution of bortrifluoride, was applied for esterification. Fatty acid methyl esters were determined by gas chromatography with flame-ionization detection.
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Analýza biologicky aktivních látek moderními separačními metodami / Analysis of biologically active substances by modern separation methodsBierhanzl, Václav January 2018 (has links)
The thesis is dedicated to the phospholipids and their polar headgroups analysis by gas chromatography, capillary electrophoresis and mass spectrometry. Phospholipids are the most important polar lipids and they are classified into phospholipid classes according to their phosphorylated groups. Phospholipids can be found in cell membranes and the changes in their ratio are monitored to research the impact of external conditions on cells. Actually thin layer chromatography is still used for phospholipid class ratio analyses. It is not suitable for microbiological research due to its time demandingness. The presented compendium of papers engaged in phospholipid classification is targeted on Bacillus subtilis strain, which produces potential antibiotics with detergent effect - surfactin. Published methods can be used for research of optimal conditions for producing microbe cultivation. Because non-polar parts of the phospholipid molecule (fatty acids) can affect the analysis methods on spliced polar headgroups have to be designed. Capillary electrophoresis and gas chromatography methods were developed and the latter one was further optimized for simultaneous analysis with fatty acids. Additional part deals with an alternative approach which consists in direct injection on mass spectrometer of intact...
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Analysis of Aroma Constituents in Cultivated Strawberries by GC/MSSong, Xiling 08 June 1999 (has links)
In aroma analysis, strawberries have always been the favored fruit because of their relatively high content of typical and pleasant aroma constituents. Esters, aldehydes, alcohols and sulfur compounds have been found to be the main aroma components in strawberry. In recent years, two volatile compounds, 2,5-dimethyl-4-methoxy-3(2H)-furanone (DMF) and 2,5-dimethyl-4-hydroxy-3(2H)-furanone (DHF) were reported to contribute heavily to strawberry aroma. These two compounds have been found in all wild strawberries studied, but found only in few cultivated varieties.
In this work, three kinds of cultivated strawberries were sampled and analyzed. The three strawberries all belong to the Camarosa variety. They came from different growing areas: Salinas (California), Orrville (Ohio), and Memphis (Tennessee). The volatile compounds of these three strawberries were separated by Gas Chromatography (GC), and identified by Mass Spectrometer Detector (MSD). Column and experimental conditions were optimized for this particular separation.
Salinas, Orrville and Memphis strawberries have very similar aroma constituents, however, in slightly differing amounts. Several unique peaks were found in each strawberry, which may well account for the differences in the aroma qualities of the three. 2-Furaldehyde was found in both Memphis and Orrville strawberries, but not in Salinas. It is a key odor compound correlated with woody aroma and it has a low odor threshold value. These two properties make it contribute negatively to the pleasant aroma of Memphis and Orrville strawberries.
A compound, 2-furanmethanol, was found only in Salinas strawberries. This compound has a faint burning aroma, however, its high odor threshold value offsets its potentially bad aroma. DMF was found in all three strawberries, but no DHF was detected in any of the three. We propose a possible explanation for the absence of DHF. Ethyl (methylthio) acetate, which is a sulfur-containing compound, was found in both Orrville and Salinas strawberries. This work is the first to report its presence in strawberries of any variety.
An external standard method was employed to quantify seven main aroma components found in the strawberry extracts. Aroma values were introduced and then calculated together with sensory descriptions of these compounds. Salinas strawberry was found to have the best aroma quality of the three. These results indicate that the odors of strawberries of the same variety can be different when grown in different geographical areas. / Master of Science
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Design and implementation of gas chromatography-mass spectrometry (GC-MS) methodologies for the analysis of thermally labile drugs and explosivesAsh, Jordan R. 18 November 2016 (has links)
Indiana University-Purdue University Indianapolis (IUPUI) / Gas Chromatography/Mass Spectrometry (GC/MS) is an analytical technique that sees frequent use in labs across the world. It is also one of the most common instruments found in forensic science laboratories. This technique can efficiently and accurately separate and identify a broad range of compounds that may be present in evidence submitted for analysis. In this work, the versatility of this instrument was applied to new methodologies for the detection of explosives and illicit drugs.
The analysis of explosives by GC/MS is common but can be problematic. The thermally sensitive nature of some explosives can cause them to degrade when introduced to the high temperatures of a GC/MS inlet. This project looked at the design and implementation of a way to separate and detect a variety of nitrate ester explosives in a short amount of time. In addition to this, a new technique known as Total Vaporization-Solid Phase Microextraction (TV-SPME) was utilized as a pre concentration technique. The parameters for TV-SPME were statistically optimized for a
low level of detection. The combination of these areas allowed for the separation of ethylene glycol dinitrate, nitroglycerin, erythritol tetranitrate, and pentaerythritol tetranitrate with a detection limit as low as 50 parts per trillion (ppt). Degradation products such as 1-mononitroglycerin, 1-3-dinitroglycerin, and 2-mononitroglycerin were also successfully identified.
The problem of thermally labile compounds extends to the world of illicit drugs. In the second project, several derivatization schemes were developed for common controlled substances. N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) was used for silylation, trifluoroacetic anhydride (TFAA) was sued for acylation, and (N,N-Dimethylformamide dimethyl acetal (DMF-DMA) for alkylation. Three different compound classes totaling 15 different drugs were investigated. N,N-Dimethylformamide dimethyl acetal (DMF-DMA) is presented as a novel way of derivatizing several drugs of interest. Primary amines and zwitterions were derivatized with this reagent to much success, specifically: amphetamine, 2-(4-Iodo-2,5-dimethoxyphenyl)ethan-1-amine (2C-I), pregabalin, and gabapentin.
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Novel One-Pot Syntheses of Uracils and Arylidenehydantoins, and Analysis of Xylitol in Chewing Gum by Gc-MsRajapaksha, RM Suranga Mahesh 06 May 2017 (has links)
The first section of this dissertation (Chapter I-III) describes the development of new methodologies to prepare uracil and arylidenehydantoin derivatives. A regioselective synthesis of 6-alkyl- and 6-aryluracils was developed by the dimerization of 3-alkyl- and 3-aryl-2-propynamides promoted by either Cs2CO3 or K3PO4. A range of 3-aryl-2- propynamides, with both electron-deficient and electron-rich 3-aryl substituents, were successfully reacted in high yields. A synthetic route to prepare arylidenehydantoins was developed using the Pd-catalyzed dimerization of 3-aryl-2-propynamides. Both electron rich and electron deficient 3-aryl-2-propynamides were dimerized successfully to produce the desired arylidenehydantoins in moderate to excellent yields. The second section of this dissertation (Chapter IV and V) describes the development of a reliable low-cost method to determine amounts of xylitol in sugar free gum samples to predict dangerous exposure levels for dogs. Xylitol is generally considered safe for human consumption and is frequently used in sugar free gum, however, it is extremely toxic to dogs. It is unknown if partially consumed chewing gum is also dangerous. A method to determine xylitol content of these sugar free gum samples employing GC-MS with direct aqueous injection (DAI) is presented. This method was successfully applied to over 120 samples including, fresh gum, 5 min, 15 min, and 30 min chewed gum samples. Further extension of this work resulted in the development of an undergraduate laboratory experiment for upper-level undergraduate chemistry students which teaches calibration methods, xylitol extraction, sample preparation for GC-MS analysis, and data analysis.
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Cílená analýza a metabolismus mastných kyselin u myší a lidí / Targeted analysis and metabolism of fatty acids in mice and humansOseeva, Marina January 2021 (has links)
Widespread sedentary lifestyle and unhealthy eating habits in the last few decades have resulted in a dramatic increase of the number of people affected by obesity, type 2 diabetes, and cardiovascular diseases. The study of these pathological conditions revealed that impaired metabolism often causes these disorders. Lipid metabolism research has contributed significantly to determining mechanisms underlying metabolic disorders. Omega-3 fatty acids are an interesting target for lipidomics studies because they were shown to lower risk of cardiovascular diseases and are hypothesized to regulate lipid metabolism. In this work, I optimized lipid extraction and chemical modification methods for analysis of fatty acids profile of tissue samples and biofluids using comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GCxGC-MS). At first, I evaluated the relative amount of omega-3 fatty acids in red blood cells (Omega-3 index) of people living in Czech Republic in either the capital city (n=476) or the rural region (n=388). For this large-scale project, I extracted phospholipids from red blood cell (RBC) membranes, transesterified them into fatty acid methyl esters (FAMEs), and measured their profile by GCxGC-MS. The mean Omega-3 index was 3.56 mol % and I detected no significant...
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Computer Aided Analysis of Gas Chromatographic SpectraRebane, Eddie 12 1900 (has links)
<p> In this thesis, hardware and software was developed
whereby the feasability of using pattern recognition
techniques for gas chromatography could be quantitively
explored. Processing methods were developed to overcome ~he
distortion inherent in GC spectra. The reproducibility of
peak retention times and areas was investigated from the
processed spectra. Upon completion of this study, it was
possible to amass a large quantity of experimental data for
bacterial strains. With such data the exact form of the
pattern recognition algorithm could be defined. A possible
pattern recognition method is discussed. </p> / Thesis / Master of Engineering (MEngr)
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Development of fuel and valueded chemicals from pyrolysis of wood/waste plastic mixtureBhattacharya, Priyanka 15 December 2007 (has links)
Highly oxygenated compounds in bio-oil produce negative properties that have hampered fuel development. Copyrolysis with plastics has increased hydrogen content in past research. Py-GC/MS analyses for two wood types (pine and oak) and three plastic types (polystyrene, polypropylene and high density polyethylene) established temperature, heating rate and residence time to produce a typical bio-oil. Analysis of various plastics to wood ratios by Py-GC/MS showed that a 50:50 wt/wt ratio produced the highest level of low molecular weight compounds best for fuel viscosity. Copyrolysis was performed on a laboratory-scale reactor at these temperature and wood-to-plastic ratios. Copyrolysis lowered bio-oil oxygen content and increased carbon content. Lower water content, acid value and viscosity also resulted, improving bio-oil suitability for fuels. Cross reactions between wood and plastics formed no new chemical species during copyrolysis. These results indicate that copyrolysis of waste plastics with woody biomass has potential for improving bio-oil properties for fuels production.
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Development and Comparison of 17beta-Estradiol Sorption Isotherms for Three Agriculturally Productive Soils From Different Physiographic Regions in VirginiaKozarek, Jessica Lindberg 10 May 2006 (has links)
Natural steroid estrogens such as 17beta-estradiol in low nanogram per liter concentrations can adversely affect the reproductive health of aquatic organisms. The overall goal of this research was to quantify the sorption of 17beta-estradiol to three soils considered to be agriculturally productive from different physiographic regions in Virginia to aid in modeling the concentration of estrogens available for transport in runoff from agricultural fields.
Batch equilibrium experiments were conducted with various concentrations of 17beta-estradiol (E2) in a background solution of 5 mM calcium chloride and 100 mg/L sodium azide added to four separate soil samples representative of productive agricultural soils from three different physiographic regions of Virginia. Groseclose loam, Myatt sandy loam and Cecil loam were supplied by the Crop and Soil Environmental Sciences Department at Virginia Tech. All soils were collected from the plow layer (0 to 15 cm) except for an additional Cecil soil sample from the Bt horizon. The concentration of E2 in the liquid phase was measured by gas chromatography/mass spectrometry (GC/MS) and was used to find the time to reach equilibrium and to develop sorption isotherms for each soil.
The time required to reach equilibrium for all soils was less than 24 hours. A linear isotherm provided the best fit to model the sorption of E2 to Cecil and Myatt soils (R2 = 0.94 and 0.96, respectively). For Groseclose soil, the general form of the Freundlich isotherm fit best (R2 = 0.98), although the linear isotherm also provided a good fit (R2 = 0.93). The sorption of E2 to agricultural soil appears to be related to the organic carbon content of each soil (Pearson coefficient, 0.82). Attempts to analyze and create isotherms for conjugated E2 by deconjugating with metholysis were unsuccessful. / Master of Science
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Volatile Compounds in Vine Tea (Ampelopsis grossedentata)Vieira Carneiro, Renata Caroline 29 June 2016 (has links)
Vine tea (Ampelopsis grossedentata) is a Chinese herbal tea, rich in the natural antioxidant dihydromyricetin, that has multiple health properties and potential food and beverage applications. However, there is little information available on vine tea aroma, color and sensory characteristics. In this study, volatile components of vine tea infusions were identified by headspace solid-phase micro-extraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Commercial vine teas samples were brewed with distilled water and Blacksburg (VA, USA) tap water and analyzed in triplicate. Vine tea infusions had acidic pH values and dark, reddish-yellow color. Type of water and vine tea sample both affected the overall volatile chemical composition of vine tea infusions. A total of fifty-six volatile components were identified in vine tea infusions. However, only seven aldehydes (hexanal, (E)-2-hexenal, (Z)-4-heptenal, nonanal, (E,Z)-2,4-heptadienal, (E,E)-2,4-heptadienal, and β-cyclocitral), two ketones (6-methyl-5-hepten-2-one and β-ionone), and one alcohol (1-penten-3-ol) were identified in more than 90% of all vine tea infusions (n=54). Results of this study may help further investigations in chemical and sensorial characteristics of vine tea, and the development of new healthy products. / Master of Science in Life Sciences
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