Brožura se zaměřuje na výzkumnou činnost Ústavu analytické chemie AV ČR. Určeno odborné veřejnosti.

• Klíčová slova
• Praha (Česko),
• MeSH
• akademie a ústavy MeSH
• analytická chemie MeSH
• chemie dějiny   MeSH
• dějiny 20. století MeSH
• dějiny 21. století MeSH
• věda MeSH
• výzkum MeSH
• Check Tag
• dějiny 20. století MeSH
• dějiny 21. století MeSH
• Geografické názvy
• Česká republika MeSH

• Konspekt
• Analytická chemie
• NLK Obory
• chemie, klinická chemie
• věda a výzkum
• NLK Publikační typ
• brožury

• O autorovi
• Ústav analytické chemie (Akademie věd ČR) Autorita

Analysis of dried urine spots (DUSs) is becoming an emerging technique in clinical, toxicological, and forensic chemistry due to the fully non-invasive collection, facile transportation, and simple storage of DUS samples. Correct DUS collection and elution is of the utmost importance because inadequate DUS sampling/processing may have direct consequences on quantitative DUS analyses and these aspects were, for the first time, comprehensively investigated in this contribution. Various groups of endogenous and exogenous species were selected as model analytes and their concentrations were monitored in DUSs collected on standard cellulose-based sampling cards. Strong chromatographic effects were observed for most analytes having a crucial impact on their distribution within the DUSs during sampling. Concentrations of target analytes were up to 3.75-fold higher in the central DUS sub-punch in comparison to the liquid urine. Consequently, substantially reduced concentrations of these analytes were determined in peripheral DUS sub-punches demonstrating that sub-punching, often applied to dried material spots, is not acceptable for quantitative DUS analyses. Hence, a simple, rapid, and user-friendly procedure was suggested, which employed an in-vial collection of a known urine volume on a pre-punched sampling disc (using a low-cost micropipette designed for patient-centric clinical sampling) and in-vial processing of the whole DUS. Excellent accuracy (0.20%) and precision (0.89%) of liquid transfers were achieved by the micropipette, which was also applied to remote DUS collection by laic and expert users. The resulting DUS eluates were analysed by capillary electrophoresis (CE) for the determination of endogenous urine species. The CE results demonstrated no significant differences between the two user groups, elution efficiencies of 88-100% (in comparison to the liquid urine), and precision better than 5.5%.

• MeSH
• lidé MeSH
• odběr biologického vzorku * MeSH
• tělesné tekutiny * MeSH
• test suché kapky krve metody   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

Direct analysis of complex samples is demonstrated by the at-line coupling of hollow fiber liquid-phase microextraction (HF-LPME) to capillary electrophoresis (CE). The hyphenation of the preparative and the analytical technique is achieved through a 3D-printed microextraction device with an HF located in a sample vial of a commercial CE instrument. The internal geometry of the device guides the CE separation capillary into the HF and the CE injection of the HF-LPME extract is performed directly from the HF lumen. The 3D-printing process ensures uniform dimensions of the devices, their constant position inside the sample vial, and excellent repeatability of the HF-LPME as well as the CE injection. The devices are cheap (∼0.01 €) and disposable, thus eliminating any possible sample-carryover, moreover, the at-line CE analysis of the extract is performed fully autonomously with no need for operator's intervention. The developed HF-LPME/CE-UV method is applied to the determination of acidic drugs in dried blood spot and wastewater samples and is characterized by excellent repeatability (RSD, 0.6-9.6%), linearity (r2, 0.9991-0.9999), enrichment (EF, 29-97), sensitivity (LOD, 0.2-3.4 μg/L), and sample throughput (7 samples/h). A further improvement of selected characteristics of the analytical method is achieved by the at-line coupling of HF-LPME to capillary isotachophoresis (ITP) with electrospray ionization-mass spectrometry (ESI-MS). The HF-LPME/ITP-ESI-MS system facilitates enhanced selectivity, matrix-free analytical signals, and up to 34-fold better sensitivity due to the use of ESI-MS detection and additional on-capillary ITP preconcentration of the HF-LPME extracts.

• MeSH
• elektroforéza kapilární MeSH
• hmotnostní spektrometrie s elektrosprejovou ionizací MeSH
• izotachoforéza * MeSH
• léčivé přípravky * MeSH
• mikroextrakce kapalné fáze * MeSH
• Publikační typ
• časopisecké články MeSH

A fully automatic millifluidic sensing platform coupling in-line nonsupported microelectromembrane extraction (μ-EME) with electrochemical detection (ECD) is herein proposed for the first time. Exploiting the features of the second generation of flow analysis, termed sequential injection (SI), the smart integration of SI and μ-EME-ECD enables (i) the repeatable formation of microvolumes of phases for the extraction step in a membrane-less (nonsupported) arrangement, (ii) diverting the acceptor plug to the ECD sensing device, (iii) in-line pH adjustment before the detection step, and (iv) washing of the platform for efficient removal of remnants of wetting film solvent, all entirely unsupervised. The real-life applicability of the miniaturized sensing system is studied for in-line sample cleanup and ECD of diclofenac as a model analyte after μ-EME of urine as a complex biological sample. A comprehensive study of the merits and the limitations of μ-EME solvents on ECD is presented. Under the optimal experimental conditions using 14 μL of unprocessed urine as the donor, 14 μL of 1-nonanol as the organic phase, and 14 μL of 25 mM NaOH as the acceptor in a 2.4 mm ID PTFE tubing, an extraction voltage of 250 V, and an extraction time of 10 min, an absolute (mass) extraction recovery of 48% of diclofenac in urine is obtained. The proposed flow-through system is proven to efficiently remove the interfering effect of predominantly occurring organic species in human urine on ECD with RSD% less than 8.6%.

• MeSH
• diklofenak * MeSH
• lidé MeSH
• membrány umělé * MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

In the present work, a disposable microextraction device with a polyamide 6 nano-fibrous supported liquid membrane (SLM) is employed for the pretreatment of minute volumes of biological fluids. The device is placed in a sample vial for an at-line coupling to a commercial capillary electrophoresis instrument with UV-Vis detection (CE-UV) and injections are performed fully automatically from the free acceptor solution above the SLM with no contact between the capillary and the membrane. Up to 4-fold enrichment of model basic (nortriptyline, haloperidol, loperamide, and papaverine) and acidic (ibuprofen, naproxen, ketoprofen, and diclofenac) drugs is achieved by optimizing the ratio of the donor to the acceptor solution volumes (16 to 4 μL, respectively). The actual setup enables SLM extractions from less than a drop of sample and is suitable for pretreatment of scarce human body fluids. Two unique methods are reported for efficient clean-up and enrichment of the basic and acidic drugs from capillary blood (formed as dried blood spot), serum, and urine samples, which enable their determination at therapeutic and/or toxic levels. The hyphenation of the SLM extraction with CE-UV analysis provides good repeatability (RSD, 2.4-14.9%), linearity (r2, 0.988-1.000), sensitivity (LOD, 0.017-0.22 mg L-1), and extraction recovery (ER, 20-106%) at short extraction times (10 min) and with minimum consumption of samples and reagents. Graphical abstract.

• MeSH
• elektroforéza kapilární metody   MeSH
• koncentrace vodíkových iontů * MeSH
• léčivé přípravky metabolismus   MeSH
• lidé MeSH
• membrány umělé * MeSH
• mikroextrakce kapalné fáze metody   MeSH
• nanovlákna * MeSH
• reprodukovatelnost výsledků MeSH
• tělesné tekutiny chemie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

V tomto článku popisujeme případ pacientky s bolestmi v epigastriu, u níž byl diagnostikován cirkulární stenózující vřed žaludku. Dalším vyšetřením byla zjištěna CMV etiologie. Po zahájení terapie inhibitory protonové pumpy a antivirové terapie došlo k úzdravě. Orgánová manifestace CMV infekce je poměrně častou komplikací u imunokompromitovaných pacientů. U imunokompetentních pacientů bývá orgánové postižení relativně vzácné. Přesto je však nutno i na tuto etiologii pomýšlet.

This article reports a case of a female patient who presented with epigastric pain. Further investigations confirmed CMV infection as a cause of stenosing gastric ulcer. In this case treatment with a proton pump inhibitor and antivirotic treatment led to a full recovery. Orgain manifestation of CMV infection if often in immunocompromitant hosts and it is, on the contratry, relatively rare in immunocompetent adults.

• MeSH
• cytomegalovirové infekce * diagnóza   farmakoterapie   komplikace   MeSH
• Cytomegalovirus izolace a purifikace   MeSH
• dospělí MeSH
• gastritida * diagnóza   etiologie   terapie   MeSH
• lidé MeSH
• slez patologie   MeSH
• stenóza patologie   MeSH
• výsledek terapie MeSH
• Check Tag
• dospělí MeSH
• lidé MeSH
• ženské pohlaví MeSH
• Publikační typ
• kazuistiky MeSH
• práce podpořená grantem MeSH

Carbamazepine is an antiepileptic drug with a narrow therapeutic index, which requires an efficient method for blood level monitoring. Finger-prick dried blood spot (DBS) collection is an alternative microsampling technique, which is less invasive than conventional venipuncture. Paper-based molecularly imprinted-interpenetrating polymer networks (MI-IPN) were developed as blood collection devices, which allowed for selective on-spot microextraction of carbamazepine from DBS. A hybrid of homogeneous polystyrene and silica gel polymer was synthesized and coated on a Whatman® Grade 1 filter paper. Proteins and other interferences in the blood samples were eliminated by using the MI-IPN collection devices, and the resulting DBS extracts were suitable for direct injection into the capillary electrophoretic instrument. The lower limit of quantitation of 4 μg/mL in capillary blood was achieved by the sweeping-micellar electrokinetic chromatography method using a KCl-containing matrix, which was sufficient for the therapeutic drug monitoring purposes. Method accuracies were in the range of 88.4 ± 4.5% to 94.5 ± 2.7% with RSD values ≤ 5.1%. The developed paper-based MI-IPN provided superior extraction efficiencies (92.2 ± 2.5%) in comparison with commercially available DBS collection cards, i.e., Whatman® 903 protein saver card (59.8 ± 2.8%) and GenCollect™ 2.0 card (47.2 ± 1.4%). The paper-based MI-IPN devices for DBS collection and on-spot extraction were characterized by simple fabrication, low costs, disposability, and reduction in sample preparation steps, and their further developments might open new perspectives in clinical applications, such as in therapeutic drug monitoring. Graphical abstract.

• MeSH
• antikonvulziva krev   izolace a purifikace   MeSH
• elektroforéza kapilární metody   MeSH
• karbamazepin krev   izolace a purifikace   MeSH
• lidé MeSH
• mikroextrakce na pevné fázi metody   MeSH
• molekulárně imprintované polymery chemie   MeSH
• monitorování léčiv MeSH
• odběr vzorku krve metody   MeSH
• papír MeSH
• tandemová hmotnostní spektrometrie MeSH
• test suché kapky krve metody   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

The effect of membrane thickness on extraction performance was systematically examined in extractions through supported liquid membranes (SLM), which were in-line coupled to capillary electrophoresis (CE). Three porous polypropylene membranes with different thickness (25, 100 and 170 μm) were used as supports for SLM extractions of model basic drugs (nortriptyline, papaverine, haloperidol and loperamide) from complex samples. The analytes were transferred through the SLMs by a pH gradient and were in-line injected, separated and quantified using a commercial CE instrument with ultraviolet (UV) detection. Transfers of the model drugs through SLM decreased with the increased membrane thickness (in the order: 25 > 100 > 170 μm) and highest transfers were achieved for the thinnest membrane. Interferences from complex sample matrices were efficiently eliminated, moreover, impregnation of the 25 μm membrane required significantly reduced volume of organic solvent. Mechanical stability of the impregnated 25 μm membrane was excellent during in-line injections, which necessitated direct contact of CE separation capillary with the SLM. Repeatability of the hyphenated SLM-CE-UV method (using the 25 μm membrane) was lower than 11% (RSD values of peak areas) and calibration curves were strictly linear in 0.5-30 μg/mL concentration range (coefficients of determination ≥ 0.997). Transfers of the basic drugs from donor solutions (standard and undiluted human urine/plasma) through the SLMs ranged from 45 to 231% and limits of detection were between 0.02 and 0.15 μg/mL.

• MeSH
• analýza moči přístrojové vybavení   metody   MeSH
• biochemická analýza krve přístrojové vybavení   metody   MeSH
• elektroforéza kapilární * MeSH
• lidé MeSH
• membrány umělé * MeSH
• rozpouštědla chemie   MeSH
• tělesné tekutiny chemie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

Planar polyamide 6 nanofibrous membrane was for the first time used in direct coupling of supported liquid membrane (SLM) extraction to CE analysis. Disposable microextraction device with the nanofibrous membrane was preassembled and stored for immediate use. The membrane in the device was impregnated with 1 µL of 1-ethyl-2-nitrobenzene and the device was subsequently filled with 10 µL of acceptor solution (10 mM HCl) and 15 µL of donor solution (sample). The device was in-line coupled to CE system for selective extraction and direct injection, separation and quantification of model basic drugs (nortriptyline, haloperidol, loperamide and papaverine) from standard saline solutions (150 mM NaCl) and from undiluted human body fluids (urine and blood plasma). Compared to standard polypropylene supporting material, the nanofibrous membrane demonstrated superior characteristics in terms of lower consumption of organic solvents, constant volumes of operational solutions, full transparency and possibility to preassemble the devices. Extraction parameters were better or comparable for the nanofibrous vs. the polypropylene membrane and the hyphenated SLM-CE method with the nanofibrous membrane was characterized by good repeatability (RSD ≤ 11.3%), linearity (r2 ≥ 0.9953; 0.5-20 mg/L), sensitivity (LOD ≤ 0.4 mg/L) and transfer (27-126%) of the basic drugs.

• MeSH
• chemické modely MeSH
• design vybavení MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• léčivé přípravky krev   izolace a purifikace   moč   MeSH
• lidé MeSH
• lineární modely MeSH
• membrány umělé * MeSH
• nanovlákna chemie   MeSH
• reprodukovatelnost výsledků MeSH
• senzitivita a specificita MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH

OBJECTIVE: To evaluate the efficacy and the learning curve of the endoscopic ultrasound-guided fine needle aspiration biopsy (EUS-FNAB) diagnostics of pancreatic lesions over 8 years (2007-2014). MATERIAL AND METHODS: EUS-FNAB using a Linear Echoendoscope Olympus was performed in 531 patients, mostly without rapid on-site evaluation (ROSE). Smears plus cytoblock sections were used routinely. Immunocytochemistry was utilised as indicated. RESULTS: The average, satisfactory sampling rate increased from the 61.2% in the first 3-year period to 72.9% in the last 3-year period (P = 0.008). The availability of the material for cytoblocks increased from 36.4% in the first period to 75.3% in the last period (P = 0.017). The efficacy of cytoblocks increased from 39.6% to 46.2% (P = 0.086). Comparing the first and last 3-year periods, the indication for immunocytochemistry did not rise substantially (5.2% and 8.5% respectively), but the predictive value of immunocytochemistry rose from 56.3% to 100.0% (P = 0.001). The most frequent diagnostic result was malignancy confirmation - both primary (41.2%) and metastatic (2.1%). In cases with representative samples and follow-up information, the specificity, sensitivity, positive predictive value and accuracy were high from the beginning. The negative predictive value decreased slightly in the last 3-year period. CONCLUSION: The pancreatic EUS-FNAB without ROSE represents a suboptimal arrangement conditioned with our staff/time/location reality. Nevertheless, within the last 3 years of our activity, nearly three-quarters of patients profit from the diagnostic contribution of this procedure.

• MeSH
• biopsie tenkou jehlou pod endosonografickou kontrolou * metody   MeSH
• dospělí MeSH
• endosonografie metody   MeSH
• imunohistochemie metody   MeSH
• jehlová biopsie metody   MeSH
• lidé středního věku MeSH
• lidé MeSH
• mladý dospělý MeSH
• nádory slinivky břišní diagnóza   patologie   MeSH
• pankreas patologie   MeSH
• prediktivní hodnota testů MeSH
• retrospektivní studie MeSH
• senioři nad 80 let MeSH
• senioři MeSH
• senzitivita a specificita MeSH
• Check Tag
• dospělí MeSH
• lidé středního věku MeSH
• lidé MeSH
• mladý dospělý MeSH
• mužské pohlaví MeSH
• senioři nad 80 let MeSH
• senioři MeSH
• ženské pohlaví MeSH
• Publikační typ
• časopisecké články MeSH