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Hollow fibre-liquid phase microextraction of basic drugs from dried dried blood spots
Dvořák, Miloš ; Miková, B. ; Šlampová, Andrea ; Kubáň, Pavel
Hollow fibre-liquid phase microextraction (HF-LPME) was applied for rapid and efficient extraction of basic drugs from dried blood spots (DBS). Basic drugs from DBS were first extracted into 10 mM NaOH solution, which acted as the HF-LPME donor solution, and simultaneously the neutralized drugs were transferred across the HF and preconcentrated in 10 mM HCl acceptor solution inside the HF lumen. Mixture (1:1, v:v) of 1-ethyl-2-nitrobenzene and dihexyl ether was used for impregnation of the porous HF membrane. Analytes in the acceptor solution were injected directly from the HF into capillary electrophoresis instrument for further separation, detection and quantification. Repeatability of the hyphenated analytical system ranged from 9.8 to 13.8 % (RSD) and enrichment factors of 52 – 78 were obtained for model basic drugs spiked to DBS extracts at a concentration level of 0.1 mg/L.
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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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Capillary electrophoresis with contactless conductivity detection for rapid determination of meldonium in urine
Šlampová, Andrea ; Kubáň, Pavel
A simple, rapid and cheap capillary electrophoresis-capacitively coupled contactless\nconductivity detection (CE-C4D) method for determination of meldonium (MEL) in\nurine samples was developed. Sample pretreatment was minimized to dilution of urine\nsamples with DI water and MEL was determined by CE-C4D in background electrolyte\nconsisting of 2 M acetic acid (pH 2.3) in ng mL−1 to mg mL−1 concentration range.\nSample-to-sample analysis time was less than 4 min, limit of detection and\nquantification was 0.015 and 0.05 μg mL−1, respectively, and the method showed\nexcellent linearity (r2 ≥ 0.9998), recovery (97.6–99.9%) and intraday as well as interday\nrepeatability (RSD ≤ 4.7%).
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