ORCID Profile
0000-0001-9960-8064
Current Organisation
University of Tasmania
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Publisher: American Chemical Society (ACS)
Date: 08-12-2017
DOI: 10.1021/ACS.ANALCHEM.7B03700
Abstract: A stacking approach in capillary electrophoresis based on the reversal of the analytes' effective electrophoretic velocities at a dynamic stacking boundary formed between charged micelles (i.e., from long chain ionic surfactants) and neutral cyclodextrins (i.e., native α-, β-, or γ-cyclodextrin) is presented. The approach was demonstrated by the long injection of s les in a micellar solution followed by injection of a cyclodextrin solution zone, and then separation by co-electro-osmotic flow capillary zone electrophoresis. The reversal is caused by the formation of stable cyclodextrin-surfactant complexes at the boundary that significantly decreased the retention factor of the analytes in the presence of a micellar pseudostationary phase. The dynamic boundary was formed at the cyclodextrin zone as the micelles penetrated this zone. Under optimum conditions, the boundary disappears, and the stacking ends when all the micelles have electrophoretically migrated to the boundary. Cationic and anionic small molecules were enriched using oppositely charged micelles from sodium dodecyl sulfate and cetyltrimethylammonium bromide, respectively. There were 1-2 orders of concentration magnitude improvement in analyte detection, which is expected in stacking with hydrodynamic injection. The improvements in the peak signals (height/corrected area) were up to 236/445 and 101/76 for the cationic and anionic analytes tested, respectively. Linearity (r
Publisher: Elsevier BV
Date: 04-2016
DOI: 10.1016/J.CHROMA.2016.03.002
Abstract: Three-step stacking by field-enhanced s le injection (FESI), sweeping, and micelle to solvent stacking (MSS) in co-EOF capillary zone electrophoresis (CZE) is presented for anionic analytes. Long FESI produced an overloaded stacked zone of analytes (four model penicillins). Sweeping of the FESI zone was by electrokinetic injection of cetyltrimethylammonium bromide (CTAB) micelles. MSS was by short injection of 60% methanol that released the swept analytes from CTAB micelles. The sensitivity enhancement factors were 146-279 and 519-954 for conductivity ratio of 10 and 100, respectively. The SEF enhancement factors (factor=SEF from three-step stacking/SEF from FESI) were 16-32 and 6-10, correspondingly. The LODs were between 6.6-13.2 ng/mL, repeatability (intraday and interday) was %RSD≤5.4%, and linearity was R(2)≥0.998. Application to real s le was investigated using fortified plasma after liquid-liquid extraction.
Publisher: MDPI AG
Date: 24-03-2019
DOI: 10.3390/MOLECULES24061166
Abstract: Urinary pterins have been found as potential biomarkers in many pathophysiological conditions including inflammation, viral infections, and cancer. However, pterins determination in biological s les is difficult due to their degradation under exposure to air, light, and heat. Besides, they occur at shallow concentration levels, and thus, standard UV detectors cannot be used without additional s le preconcentration. On the other hand, ultra-sensitive laser-induced fluorescence (LIF) detection can be used since pterins exhibit native fluorescence. The main factor that limits an everyday use of LIF detectors is its high price. Here, an alternative detector, i.e., light-emitted diode induced fluorescence (LEDIF) detector, was evaluated for the determination of pterins in urine s les after capillary electrophoresis (CE) separation. An optimized method was validated in terms of linearity range, limit of detection (LOD), limit of quantification (LOQ), intra- and interday precision and accuracy, s le stability in the autos ler, and s le stability during the freezing/thawing cycle. The obtained LOD (0.1 µM) and LOQ (0.3 µM) values were three-order of magnitude lower compared to UV detector, and two orders of magnitude higher compared to previously reported house-built LIF detector. The applicability of the validated method was demonstrated in the analysis of urine s les from healthy in iduals and cancer patients.
Publisher: Elsevier BV
Date: 04-2017
DOI: 10.1016/J.JPBA.2017.01.032
Abstract: Urinary tract infection (UTI) is one of the most common bacterial infection in human but its diagnosis is difficult. Metabolomic studies with nuclear magnetic resonance of urine have shown that acetic acid/creatinine ratio may be used for early UTI diagnosis. Here, a method for simultaneous determination of acetate and creatinine by capillary zone electrophoresis with contactless conductivity detector was developed for the first time. The separation was with 40mM MES and 20mM l-histidine as a background solution. The total time of a single run, including capillary conditioning, was less than 12min. The method was successfully demonstrated for analysis of actual and fortified human urine s les after methanol dilution. Analytical figures of merit such as linearity, LOQ, and repeatability (intraday and interday) were studied.
Publisher: Elsevier BV
Date: 12-2015
DOI: 10.1016/J.CHROMA.2015.10.089
Abstract: The sensitivity enhancement factor (SEF) in field enhanced s le injection (FESI) in capillary electrophoresis is dictated by the conductivity ratio. The higher the conductivity ratio (using very low conductivity s le diluents such as water), the higher the SEF. Here, we improved the performance of FESI by combination with sweeping and micelle to solvent stacking (MSS) in a well-defined three-step stacking procedure using model cationic drugs. The separation was by capillary zone electrophoresis (CZE) using 100mM phosphoric acid as background solution (BGS). Under the experimental conditions studied, the SEF (vs. typical injection in CZE) range of FESI using a conductivity ratio of 10, 100, and 1000 (s le diluent with conductivity 10, 100, and 1000× lower than the BGS, respectively) was 5-6, 33-50, and 272-393, respectively. The SEF range of three-step stacking was 308-891, 2188-6463, and 3088-6499, correspondingly. The SEF enhancement factor due to three-step stacking (SEF of three-step stacking ided by SEF of FESI) was from 11 to 161. We evaluated the performance of proposed procedure using a conductivity ratio of 10 (10mM phosphoric acid as diluent) which is the minimum requirement for field-enhancement. The strategy was as follows: long FESI (e.g., 420s at 10kV) to form an overloaded stacked zone sweeping (e.g., 315s at -10kV) with 10mM sodium dodecyl sulfate micelles and MSS by injection (6s at 50mbar) of 30% acetonitrile. The strategy was studied in terms of sweeping and MSS conditions, FESI/sweeping time ratio, and FESI time at constant FESI/sweeping ratio. Analytical figures of merit including linearity, LOD (S/N=3), and repeatability (intraday and interday) were determined. Moreover, s le matrix effect was studied using acetone treated plasma s le.
Publisher: Wiley
Date: 07-11-2014
Abstract: Multidimensional separation where two or more orthogonal displacement mechanisms are combined is a promising approach to increase peak capacity in CE. The combinations allow dramatic improvement of analytical performance since the total peak capacity is given by a product of the peak capacities of all methods. The initial reports were concentrated on the construction of effective connections between capillaries for 2D analysis. Today, 2D and 3D CE systems are now able to separate real complex biological or environmental mixtures with good repeatability, improved resolution with minimal loss of s le. This review will present the developments in the field of multidimensional CE during the last 15 years. The endeavors in this specific field were on the development of interfaces, interface-free techniques including integrated separations, microdevices, and on-line s le concentration techniques to improve detection sensitivity.
Publisher: Royal Society of Chemistry (RSC)
Date: 2016
DOI: 10.1039/C5AY02493E
Abstract: In the last decade, capillary electrophoresis (CE) has joined other analytical separation techniques that are widely used in metabolomics.
No related grants have been discovered for Wojciech Grochocki.