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Coupling of micro-electromembrane extraction to transient capillary isotachophoresis for the analysis of drugs in biological samples
Lučaj, Martin ; Pospíchal,, Jan (oponent) ; Dvořák, Miloš (vedoucí práce)
The diploma thesis is focused on the development of in-line micro-electromembrane extraction (EME) coupled to capillary electrophoresis (CE) for the analysis of selected drugs in body fluids. Up to now, direct coupling of EME to CE has been demonstrated on diluted river samples only [1]. Although the published set-up has been implemented within a commercial CE it suffers from several drawbacks that can have a negative impact on the analysis of samples with higher complexity. The instrumental arrangement presented in this thesis eliminates these deficiencies. The experimental part is based on the optimization of fundamental extraction and separation conditions for the analysis of model basic drugs (nortriptyline, haloperidol, loperamide) with the use of transient isotachophoresis (tITP) principle. The extraction conditions were optimized for electro-driven transport of basic analytes from complex matrices (urine) through free liquid membrane followed by injection step utilized by electrokinetic supercharging (EKS), which focused target analytes into the CE capillary. Optimized conditions have been applied on blood in the form of dry blood spots, which are highly attractive samples in the current clinical analysis. The repeatability of the measurements was
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Application of microextraction techniques for analysis of biological samples
Lučaj, Martin ; Vespalcová, Milena (oponent) ; Dvořák, Miloš (vedoucí práce)
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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Coupling of micro-electromembrane extraction to transient capillary isotachophoresis for the analysis of drugs in biological samples
Lučaj, Martin ; Pospíchal,, Jan (oponent) ; Dvořák, Miloš (vedoucí práce)
The diploma thesis is focused on the development of in-line micro-electromembrane extraction (EME) coupled to capillary electrophoresis (CE) for the analysis of selected drugs in body fluids. Up to now, direct coupling of EME to CE has been demonstrated on diluted river samples only [1]. Although the published set-up has been implemented within a commercial CE it suffers from several drawbacks that can have a negative impact on the analysis of samples with higher complexity. The instrumental arrangement presented in this thesis eliminates these deficiencies. The experimental part is based on the optimization of fundamental extraction and separation conditions for the analysis of model basic drugs (nortriptyline, haloperidol, loperamide) with the use of transient isotachophoresis (tITP) principle. The extraction conditions were optimized for electro-driven transport of basic analytes from complex matrices (urine) through free liquid membrane followed by injection step utilized by electrokinetic supercharging (EKS), which focused target analytes into the CE capillary. Optimized conditions have been applied on blood in the form of dry blood spots, which are highly attractive samples in the current clinical analysis. The repeatability of the measurements was
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Application of microextraction techniques for analysis of biological samples
Lučaj, Martin ; Vespalcová, Milena (oponent) ; Dvořák, Miloš (vedoucí práce)
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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