A capillary system formed by combining 25 and 100 μm id capillaries was used in the short-end injection mode to determine creatinine and uric acid in human urine. The separation was performed at an electric field intensity of 2.3 kV/cm. Creatinine was determined in a BGE with a composition of 20 mM citric acid/NaOH (pH 3.0), and uric acid was determined in 20 mM MES/NaOH (pH 6.0). Under these conditions, migration times of 12.2 s for creatinine and 8.6 s for uric acid were achieved. The LOD value is 2.4 mg/L for creatinine and 0.9 mg/L for uric acid; the RSD for the migration time varies in the range 0.7-1.1% (intra day) to 1.0-7.5% (inter day); RSDs for the peak areas equalled 3.4-4.0% (intra day) and 4.3-4.7% (inter day). The determined creatinine values in seven urine samples vary in the range 221-1394 mg/L for creatinine and 87-615 mg/L for uric acid. t-Test did not reveal any statistically significant difference between the developed CE methodologies and reference methods - Jaffé reaction for creatinine and enzymatic uricase test for uric acid.

• Klíčová slova
• Capillary electrophoresis, Clinical analysis, Creatinine, High-speed analysis, Uric acid,
• MeSH
• časové faktory MeSH
• dospělí MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• kreatinin moč   MeSH
• kyselina močová moč   MeSH
• lidé MeSH
• limita detekce MeSH
• lineární modely MeSH
• reprodukovatelnost výsledků MeSH
• Check Tag
• dospělí MeSH
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• kreatinin MeSH
• kyselina močová MeSH

GC with nitrogen phosphorus detection and HPLC with UV detection were used to determine midazolam (MDZ) levels in rabbit plasma following ocular and nasal administration. For GC with nitrogen phosphorus detection, the analyte was extracted from the plasma using a three-step liquid-liquid extraction including extraction with an isopropanol/butyl chloride mixture in an alkaline solution, followed by extractions with 1 M HCl, and finally with an alkaline solution of butyl chloride. The recovery of MDZ was dependent on the sample alkalization time prior to the final extraction. The procedure increased the recovery of MDZ up to 99.6%. Improved sample preparation led to a significant increase in the sensitivity of the determination by GC with nitrogen phosphorus detection. The achieved detection limit was 0.34 ng/mL, which is ten times lower than that obtained using HPLC with UV detection. The small plasma volume was another advantage of the GC with nitrogen phosphorus detection method (200 μL per assay). Both administration routes of the anesthetic (nasal and ocular) resulted in comparable plasma MDZ levels. Kinetic simulation of the MDZ plasma was performed for both administration routes.

• Klíčová slova
• Fentanyl, Midazolam, Nasal administration, Nitrogen phosphorus detection, Ocular administration,
• MeSH
• aplikace intranazální MeSH
• aplikace oční MeSH
• chromatografie plynová metody   MeSH
• hypnotika a sedativa aplikace a dávkování   krev   MeSH
• králíci MeSH
• limita detekce MeSH
• midazolam aplikace a dávkování   krev   MeSH
• vysokoúčinná kapalinová chromatografie metody   MeSH
• zvířata MeSH
• Check Tag
• králíci MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• hypnotika a sedativa MeSH
• midazolam MeSH

A fused-silica capillary with a common outer diameter, 360 μm, but containing seven internal channels, each 28 μm in diameter (a multichannel capillary), has been tested on electrophoretic separations of mixtures of dopamine, adrenaline, and noradrenaline, using a contactless conductivity and UV photometric detection. It has been demonstrated that the sensitivity of the detection of these neurotransmitters in multichannel capillary, in comparison with those obtained for a standard singlechannel capillary with similar cross-sectional area, is comparable to that for the contactless conductivity and is about 50% higher for the UV photometry. The sensitivity is increased without loss of the separation efficiency, in contrast to UV detection with bubble cell. Further possibilities of using a multichannel capillary are demonstrated on separations of mixtures of inorganic cations (K⁺, Ba²⁺, Na⁺, Mg²⁺, and Li⁺) and mixtures of glucose and ribose. The main advantage of multi-channel capillary in comparison with a singlechannel capillary with the same cross-sectional area becomes apparent in separations in background electrolytes of high conductivity.

• Klíčová slova
• CE, Contactless conductivity detection, Multichannel capillary, Neurotrans-mitters, UV photometry detection,
• MeSH
• adrenalin izolace a purifikace   MeSH
• design vybavení MeSH
• dopamin izolace a purifikace   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární přístrojové vybavení   MeSH
• neurotransmiterové látky izolace a purifikace   MeSH
• noradrenalin izolace a purifikace   MeSH
• senzitivita a specificita MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• adrenalin MeSH
• dopamin MeSH
• neurotransmiterové látky MeSH
• noradrenalin MeSH

A capillary formed by connecting a 9.7 cm-long separation capillary with id 25 μm with an auxiliary 22.9 cm-long capillary with id 100 μm (coupled capillary) was tested for electrophoretic separation at high electric field intensities. The coupled capillary was placed in the cassette of a standard electrophoresis apparatus. It was used in the short-end injection mode for separation of a mixture of dopamine, noradrenaline, and adrenaline in a BGE of 20 mM citric acid/NaOH, pH 3.2. An intensity of 2.7 kV/cm was attained in the separation part of the capillary at a separation voltage of 30 kV, which is 2.9 times more than maximum intensity value attainable in a capillary with the same length with uniform id. At these high electric field intensities, the migration times of the tested neurotransmitters had values of 12.3-13.3 s and the attained separation efficiency was between 2350 and 2760 plates/s. It is thus demonstrated that an effective separation instrument - a coupled capillary - can be used for very rapid separation in combination with standard, commercially available instrumentation.

• MeSH
• časové faktory MeSH
• chemické modely MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• hydroxid sodný chemie   MeSH
• katecholaminy analýza   chemie   izolace a purifikace   MeSH
• kyselina citronová chemie   MeSH
• neurotransmiterové látky analýza   chemie   izolace a purifikace   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• hydroxid sodný MeSH
• katecholaminy MeSH
• kyselina citronová MeSH
• neurotransmiterové látky MeSH

A capillary electrophoresis (CE) procedure with contactless conductivity detection (C(4)D) has been developed for monitoring of neutral mono- and disaccharides in drinks and foodstuffs. The separation of a mixture of seven neutral saccharides (glucose, fructose, galactose, mannose, ribose, sucrose and lactose) employed a quartz capillary, 5 μm i.d., with an effective length of 18.3 cm, and 75 mM NaOH (pH 12.8) as the background electrolyte (BGE). The limit of detection (LOD) values obtained lied within a range from 0.4 μmol L(-1) for lactose to 0.9 μmol L(-1) for ribose, with a separation time shorter than 140 s. The procedure was successfully applied to determinations of saccharides in fruit juices, Coca-Cola, milk, red and white wines, yoghurts, honey and a foodstuff additive.

• MeSH
• analýza potravin přístrojové vybavení   metody   MeSH
• časové faktory MeSH
• disacharidy analýza   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• limita detekce MeSH
• monosacharidy analýza   MeSH
• nápoje analýza   MeSH
• potravinářské přísady analýza   MeSH
• ribosa analýza   MeSH
• zvířata MeSH
• Check Tag
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• disacharidy MeSH
• monosacharidy MeSH
• potravinářské přísady MeSH
• ribosa MeSH

A mixture of 29 organic acids (OAs) occurring in urine was analyzed by capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C(4)D) and UV photometric detection. The optimized analytical system involved a 100 cm long polyacrylamide-coated capillary (50 μm i.d.) and the background electrolyte of 20mM 2-morpholinoethanesulfonic acid (MES)/NaOH+10% (v/v) methanol, pH 6.0 (pH is related to the 20mM MES/NaOH buffer in water). The LOD values obtained by C(4)D for the OAs which do not absorb UV radiation range from 0.6 μM (oxalic acid) to 6.8 μM (pyruvic acid); those obtained by UV photometry for the remaining OAs range from 2.9 μM (5-hydroxy-3-indoleacetic acid) to 10.2 μM (uric acid). The repeatability of the procedure developed is characterized by the coefficients of variation, which vary between 0.3% (tartaric acid) and 0.6% (5-hydroxy-3-indoleacetic acid) for the migration time and between 1.3% (tartaric acid) and 3.5% (lactic acid) for the peak area. The procedure permitted quantitation of 20 OAs in a real urine sample and was applied to monitoring of the occurrence of the inborn metabolic fault of methylmalonic aciduria.

• MeSH
• analýza moči metody   MeSH
• dospělí MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární metody   MeSH
• kalibrace MeSH
• kyseliny moč   MeSH
• lidé MeSH
• limita detekce MeSH
• mladý dospělý MeSH
• organické látky moč   MeSH
• reprodukovatelnost výsledků MeSH
• spektrofotometrie ultrafialová MeSH
• vrozené poruchy metabolismu aminokyselin diagnóza   MeSH
• Check Tag
• dospělí MeSH
• lidé MeSH
• mladý dospělý MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• kyseliny MeSH
• organické látky MeSH

CE with contactless conductivity detection has been used to separate 28 biogenic amino acids in a short capillary with an effective length of 18 cm. All the tested amino acids can be mutually separated in 0.5-10 mol/L acetic acid electrolytes. The time of analysis does not exceed 6 min and the LODs vary from 0.1 to 1.7 micromol/L. The CVs lie within the intervals 0.01-0.4% and 0.9-4% for the migration times and the analyte peak areas, respectively. The procedure has been successfully applied to the determinations of the whole amino acid spectra in blood plasma, urine, saliva and cerebrospinal fluid samples.

• MeSH
• aminokyseliny analýza   krev   mozkomíšní mok   moč   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární metody   MeSH
• lidé MeSH
• referenční hodnoty MeSH
• senzitivita a specificita MeSH
• sliny chemie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• aminokyseliny MeSH

A CE procedure employing capacitively coupled contactless conductivity detection has been developed for direct determination of the glycerol and mannitol polyalcohols in biological and pharmacological samples. Both glycerol and mannitol are fully separated from the sample matrix within very short times of 3.0 and 3.9 min, respectively, when using the optimized BGE, 60 mM H3BO3+30 mM LiOH (pH 9.1). The LODs amount to 0.5 microM for glycerol and 0.3 microM for mannitol. The repeatability of the glycerol determination in real biological materials is characterized by the coefficient of variation values, 0.5 and 3.2%, for the migration time and the peak area, respectively. The procedure has been used to monitor the free glycerol concentration in adipose tissue microdialyzates. A physiological study has demonstrated that the lipolysis occurring during a sporting action can be stimulated by local application of adrenaline. The procedure has further been utilized to determine mannitol in a pharmacological preparation.

• MeSH
• acetonitrily chemie   MeSH
• cvičení fyziologie   MeSH
• cyklistika fyziologie   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární metody   MeSH
• glycerol analýza   metabolismus   MeSH
• kalibrace MeSH
• koncentrace vodíkových iontů MeSH
• kyseliny borité chemie   MeSH
• lidé MeSH
• lineární modely MeSH
• lipolýza fyziologie   MeSH
• mannitol analýza   metabolismus   MeSH
• reprodukovatelnost výsledků MeSH
• senzitivita a specificita MeSH
• sloučeniny lithia chemie   MeSH
• tuková tkáň chemie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• acetonitrile MeSH Prohlížeč
• acetonitrily MeSH
• boric acid MeSH Prohlížeč
• glycerol MeSH
• kyseliny borité MeSH
• lithium hydroxide MeSH Prohlížeč
• mannitol MeSH
• sloučeniny lithia MeSH

CE with contactless conductivity detection has been used to determine the glycine neurotransmitter in periaqueductal gray matter (PAG) of rats. The LOD for glycine has been decreased to a value of 0.2 microM by adding 75% v/v of ACN to the samples and increasing the sample zone introduced to a value of 20% of the overall capillary length. The repeatabilities of the analyte migration times and the zone areas amount to 2.1 and 2.7%, respectively. The optimized CE/contactless conductivity detection method makes it possible to determine the micromolar concentrations of glycine in PAG microdialyzates without the necessity of sample derivatization. It follows from a pharmacological study that a local inflammation initiated by an application of carrageenan increased the glycine concentration in the rat PAG seven times, compared with a control. The glycine level in PAG can be decreased and the pain suppressed by administering paracetamol.

• MeSH
• bolest chemicky indukované   farmakoterapie   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární metody   MeSH
• glycin analýza   metabolismus   MeSH
• karagenan farmakologie   MeSH
• krysa rodu Rattus MeSH
• neopioidní analgetika farmakologie   MeSH
• paracetamol farmakologie   MeSH
• potkani Wistar MeSH
• reprodukovatelnost výsledků MeSH
• senzitivita a specificita MeSH
• substantia grisea centralis chemie   MeSH
• zvířata MeSH
• Check Tag
• krysa rodu Rattus MeSH
• mužské pohlaví MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• glycin MeSH
• karagenan MeSH
• neopioidní analgetika MeSH
• paracetamol MeSH

CE with capacitively coupled contactless conductivity detection (C(4)D) was used to determine waste products of the nitrogen metabolism (ammonia and creatinine) and of biogenic inorganic cations in samples of human urine. The CE separation was performed in two BGEs, consisting of 2 M acetic acid + 1.5 mM crown ether 18-crown-6 (BGE I) and 2 M acetic acid + 2% w/v PEG (BGE II). Only BGE II permitted complete separation of all the analytes in a model sample and in real urine samples. The LOD values for the optimized procedure ranged from 0.8 microM for Ca(2+) and Mg(2+) to 2.9 microM for NH(4)(+) (in terms of mass concentration units, from 7 microg/L for Li(+) to 102 microg/L for creatinine). These values are adequate for determination of NH(4)(+), creatinine, Na(+), K(+), Ca(2+) and Mg(2+) in real urine samples.

• MeSH
• amoniak moč   MeSH
• elektrická vodivost MeSH
• elektroforéza kapilární metody   statistika a číselné údaje   MeSH
• kationty moč   MeSH
• kreatinin moč   MeSH
• lidé MeSH
• polyethylenglykoly MeSH
• reprodukovatelnost výsledků MeSH
• roztoky MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• amoniak MeSH
• kationty MeSH
• kreatinin MeSH
• polyethylenglykoly MeSH
• roztoky MeSH