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Application of microextraction techniques for analysis of biological samples
Lučaj, Martin ; Vespalcová, Milena (referee) ; Dvořák, Miloš (advisor)
This bachelor thesis deals with the analysis of basic drugs in biological samples by in line coupling of supported liquid membrane (SLM) to capillary electrophoresis (CE). The tITP method was included as an on-line preconcentration step to achieve better detection limits with ammonium acetate as the tITP stacker and acetic acid as the CE background electrolyte. The practical part of the thesis focuses on the optimization of the tITP and the SLM extraction conditions in the analysis of basic drugs in complex biological samples (human urine). The best analytical results were achieved with hydrodynamic injection of ammonium acetate for 15 s and basic drugs for 15 s. The donor was alkalised with 10 mM sodium hydroxide and acceptor was acidified with 10 mM hydrochloric acid. From the results, the in-line coupling of SLM extraction to CE and stacking by tITP is an efficient method allowing direct analysis of complex samples with improved sensitivity of the analytical method.
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Application of microextraction techniques for analysis of biological samples
Lučaj, Martin ; Vespalcová, Milena (referee) ; Dvořák, Miloš (advisor)
This bachelor thesis deals with the analysis of basic drugs in biological samples by in line coupling of supported liquid membrane (SLM) to capillary electrophoresis (CE). The tITP method was included as an on-line preconcentration step to achieve better detection limits with ammonium acetate as the tITP stacker and acetic acid as the CE background electrolyte. The practical part of the thesis focuses on the optimization of the tITP and the SLM extraction conditions in the analysis of basic drugs in complex biological samples (human urine). The best analytical results were achieved with hydrodynamic injection of ammonium acetate for 15 s and basic drugs for 15 s. The donor was alkalised with 10 mM sodium hydroxide and acceptor was acidified with 10 mM hydrochloric acid. From the results, the in-line coupling of SLM extraction to CE and stacking by tITP is an efficient method allowing direct analysis of complex samples with improved sensitivity of the analytical method.
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ICP-OES with electrothermal vaporisation (ETV) as a possible tool for direct analysis of various biologic samples
Matějková, Stanislava
Solid sampling electrothermal vaporization (ETV) inductively coupled plasma optical emission spectroscopy (ICP-OES) enable simple and rapid multielemental analysis of major, minor and trace elements without the need for pre-treatment of solid or liquid samples. By comparison with more common ICP-OES combined with a solution nebulization, the risk of contamination of analysed samples is reduced. The detection limits and the sample quantity needed for analysis via ETV-ICP-OES decrease as a result of the high-efectivity transport of the sample aerosol into the ICP torch. The connection of ETV unit to simultaneous ICP-OES allows us the fast direct and fully automatised analysis of numerous samples. The technique enable usually the combined calibration with home-made or certified solid and aqueous standards. We developed the methodology for tracking the carboran-based candidate-drugs time dependent concentration and for their pharmacokinetic evaluation. The method is based on direct boron or together boron and cobalt contents direct estimation in little amounts of fresh frozen mice tissues (5 – 10 mg of serum, brain or liver). We created also methods for multielement analysis of plant material and for determination of potentionaly harmful elements in insect bodies.\n
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Analysis of phospholipids by comprehensive gas chromatography
Šilhavecká, Simona ; Čabala, Radomír (advisor) ; Jelínek, Ivan (referee)
Phospholipids are an important group of polar lipids constituting the main component of cell membranes. Their proportion may vary depending on many factors of the surrounding environment in which the cell is located. Determination of membrane phospholipids is essential in many scientific, industrial and economic sectors. The aim of this work has been to develop a separation method for determination of membrane phospholipids by which it was possible to analyze phosphorylated parts of phospholipids and fatty acids from one sample. Comprehensive gas chromatography with mass detection (GC×GC-MS) was chosen for the assay. This method allows the separation of the entire sample on two serially connected different columns, among which is the interface called modulator. The preparation of the sample includes a cleavage of the phospholipid molecule by the enzyme phospholipase C, which released the phosphorylated polar headgroups. These polar parts had to be derivatized before analysis. The principle of the chosen derivatization consisted in the use of two different silylation agents (hexamethyldisilazane and N,O-Bis(trimethylsilyl) trifluoracetamide) in two steps. Conditions were selected for efficient separation of the silylderivatives of phosphorylated headgroups using GC×GC-MS using a cryogenic...
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ICP-OES with electrothermal vaporisation (ETV) as a possible tool for direct analysis of biologic samples
Matějková, Stanislava
Solid sampling electrothermal vaporization (ETV) inductively coupled plasma optical emission spectroscopy (ICP-OES) enable simple and rapid multielemental analysis of major, minor and trace elements without the need for pre-treatment of solid or liquid samples. By comparison with more common ICP-OES combined with a solution nebulization, the risk of contamination of analysed samples is reduced. The detection limits and the sample quantity needed for analysis via ETV-ICP-OES decrease as a result of the high-efectivity transport of the sample aerosol into the ICP torch. The connection of ETV unit to simultaneous ICP-OES allows us the fast direct and fully automatised analysis of numerous samples. The technique enable usually the combined calibration with home-made or certified solid and aqueous standards. We developed the methodology for tracking the carboran-based candidate-drugs time dependent concentration and for their pharmacokinetic evaluation. The method is based on direct boron or together boron and cobalt contents direct estimation in little amounts of fresh frozen mice tissues (5 – 10 mg of serum, brain or liver).\n
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Micro-electromembrane extraction across multiple aqueous and organic phases for selective pretreatment of raw biological samples
Kubáň, Pavel ; Boček, Petr ; Seip, K. F. ; Gjelstad, A. ; Pedersen-Bjergaard, S.
Micro-electromembrane extraction (μ-EME) across multiple aqueous and organic\nsolutions was developed for selective extractions of various analytes from untreated\nbiological samples. The novel approach requires μL volumes of samples and organic\nsolvents, which form consecutive immiscible plugs in a transparent polymeric capillary\nand the extraction process is accelerated by application of d.c. voltage. Number of the\nplugs, their composition, volume and sequence in the extraction capillary can be chosen\nspecifically for each particular application and high variability and selectivity of the\nextraction process can be achieved. In this contribution, we demonstrate suitability of\na five-phase μ-EME system for simultaneous extractions of cations and anions from\nurine and for selective extractions of basic analytes based on their acid-base strength\nfrom plasma.
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Utilize of instrumentality PSE (Pressurized Solvent Extraction) in food analysis
Grulichová, Hana ; Vítová, Eva (referee) ; Vespalcová, Milena (advisor)
This bachelor thesis is engaged in the modern method of extraction PSE (pressurized solvent extraction). There have been two types of this apparatus, One PSE and Fast PSE. In this thesis, the apparatus and its behavior is described. Extraction of anthraquinones, strychnine, berberine, glycyrrhizin, ligustilides from medical plants is presented below. These substancies are used mainly in treatment for various diseases. In this work is noticed trace elements, tocopherols, alkylbenzene sulphonate, isoflavone, dionine, betacarotene, vitamin E, polyphenol extracted from biological samples. Utilization of the substancies from biological samples is very different. Some one decreased risk of osteoporosis, cardiovascular disease, cancer and other is by contrast deleterious toxin. High attention is devoted to substancies presented in food such as polychlorinated biphenyls, various pesticides, lipids, oxysterols. These substancies are in food rather undesirable than is why their amount is determinated to the food isn´t deleterious.
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