A review is presented on the state of the art of the chemiluminescence analysis of pharmaceuticals by the two most relevant automated controlled-flow methodologies--flow-injection analysis (FIA) and sequential-injection analysis (SIA). The current chemiluminometric applications of FIA and SIA in pharmaceutical analysis are discussed with special emphasis on the analytical figures of merit and sample matrix characteristics. The review involving 211 references and covering papers published between 2001 and 2006 is divided into several sections according to the fundamental types of chemiluminescence systems employed.

• MeSH
• léčivé přípravky analýza   MeSH
• luminiscenční měření metody   MeSH
• oxidace-redukce MeSH
• průtoková injekční analýza MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH
• Názvy látek
• léčivé přípravky MeSH

New generation of sequential injection analysis (SIA) called sequential injection chromatography (SIC) has already been consolidated as a good alternative of high performance liquid chromatography (HPLC) for fast analysis of simple samples. Benefits of flow methods are automation, miniaturization and low sample and mobile phase consumption. Implementation of short monolithic chromatographic column into SIA opens new area-on-line chromatographic separation of multi-compound sample in low-pressure flow system, with the advantage of flow programming and possibility of sample manipulation. In the presented review the potential of SIC and its comparison with HPLC for determination of pharmaceutical mixtures is discussed and outlines past and recent trends focused on separation with SIC.

• MeSH
• chromatografie přístrojové vybavení   metody   MeSH
• lékové formy MeSH
• lidé MeSH
• průtoková injekční analýza přístrojové vybavení   metody   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH
• Názvy látek
• lékové formy MeSH

This paper deals with the development of an automated procedure for formulation assays and dissolution tests based on a sequential injection analysis (SIA) system involving an ion-selective electrode as sensing device. Construction of a tubular salicylate (Sal) selective electrode suitable for potentiometric determination of acetylsalicylic acid (Asa) in pharmaceutical formulations is described. The flow-through electrode is formed by a PVC membrane containing 29.2% (w/w) PVC, 5.8% (w/w) tetraoctylammonium salicylate (ionic sensor), 58.5% o-nitrophenyloctylether (plasticizer) and 6.5% (w/w) p-tert-octylphenol (stabilising additive which increases electrode selectivity). The calibration range is 0.05--10 mM Sal, the limit of detection (LOD) is 0.05 mM Sal, the slope is 56.0 mV per decade at 22 degrees C. The R.S.D. is 0.20% (15 readings) when determining 2.5 mM Sal in standard solution. The electrode is used for sensing Asa after its on-line chemical hydrolysis to Sal in a SIA system. The sampling rate is 6 h(-1) but for the dissolution tests the frequency is increased to 20 h(-1). The SIA set-up is employed for the assay of Asa in plain tablets, composed tablets and effervescent tablets and for performing dissolution tests of normal and sustained release tablets. Results obtained by this technique compare well with those required by the US Pharmacopoeia XXIV.

• MeSH
• Aspirin analýza   MeSH
• elektrochemie přístrojové vybavení   MeSH
• elektrody * MeSH
• kalibrace MeSH
• rozpustnost MeSH
• senzitivita a specificita MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• Aspirin MeSH

Automated sequential injection (SIA) method for chemiluminescence (CL) determination of nonsteroidal anti-inflammatory drug indomethacin (I) was devised. The CL radiation was emitted in the reaction of I (dissolved in aqueous 50% v/v ethanol) with intermediate reagent tris(2,2'-bipyridyl)ruthenium(III) (Ru(bipy)(3)(3+)) in the presence of acetate. The Ru(bipy)(3)(3+) was generated on-line in the SIA system by the oxidation of 0.5mM tris(2,2'-bipyridyl)ruthenium(II) (Ru(bipy)(3)(2+)) with Ce(IV) ammonium sulphate in diluted sulphuric acid. The optimum sequence, concentrations, and aspirated volumes of reactant zones were: 15 mM Ce(IV) in 50mM sulphuric acid 41 microL, 0.5 mM Ru(bipy)(3)(2+) 30 microL, 0.4M Na acetate 16 microL and I sample 15 microL; the flow rates were 60 microLs(-1) for the aspiration into the holding coil and 100 microLs(-1) for detection. Calibration curve relating the intensity of CL (peak height of the transient CL signal) to concentration of I was curvilinear (second order polynomial) for 0.1-50 microM I (r=0.9997; n=9) with rectilinear section in the range 0.1-10 microM I (r=0.9995; n=5). The limit of detection (3sigma) was 0.05 microM I. Repeatability of peak heights (R.S.D., n=10) ranged between 2.4% (0.5 microM I) and 2.0% (7 microM I). Sample throughput was 180 h(-1). The method was applied to determination of 1 to 5% of I in semisolid dosage forms (gels and ointments). The results compared well with those of UV spectrophotometric method.

• MeSH
• indomethacin analýza   chemie   MeSH
• kalibrace MeSH
• lékové formy * MeSH
• luminiscenční měření přístrojové vybavení   metody   MeSH
• molekulární struktura MeSH
• organokovové sloučeniny * MeSH
• průtoková injekční analýza přístrojové vybavení   metody   MeSH
• reprodukovatelnost výsledků MeSH
• rozpouštědla MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• indomethacin MeSH
• lékové formy * MeSH
• organokovové sloučeniny * MeSH
• rozpouštědla MeSH
• tris(2,2'-bipyridyl)ruthenium(II) MeSH Prohlížeč

This paper deals with a novel approach to separate two analytes with different chemical properties and different lipophilicity. The newly described methodology is based on the two column system that was used for isocratic separation of two analytes with very different lipophilicity-dexamethasone and cinchocaine. Simultaneous separation of model compounds cinchocaine and dexamethasone was carried under the following conditions in two-column sequential injection chromatography system (2-C SIC). A 25×4.6 mm C-18 monolithic column was used in the first dimension for retention and separation of dexamethasone with mobile phase acetonitrile:water 30:70 (v/v), flow rate 0.9 mL min(-1) and consumption of 1.7 mL. A 10×4.6 mm C-18 monolithic column with 5×4.6 mm C-18 precolumn was used in the second dimension for retention and separation of cinchocaine using mobile phase acetonitrile:water 60:40 (v/v), flow rate 0.9 mL min(-1) and consumption 1.5 mL. Whole analysis time including both mobile phase's aspirations and both column separations was performed in less than 4 min. The method was fully validated and used for determination of cinchocaine and dexamethasone in pharmaceutical otic drops. The developed 2-C SIC method was compared with HPLC method under the isocratic conditions of separation on monolithic column (25×4.6 mm C-18). Spectrophotometric detection of both compounds was performed at wavelength 240 nm. System repeatability and method precision were found in the range (0.39-3.12%) for both compounds. Linearity of determination was evaluated in the range 50-500 μg mL(-1) and coefficients of determination were found to be r(2)=0.99912 for dexamethasone and r(2)=0.99969 for cinchocaine.

• Klíčová slova
• Cinchocaine, Dexamethasone, Sequential injection analysis (SIA), Sequential injection chromatography (SIC), Two-column sequential injection chromatography (2-C SIC),
• MeSH
• anestetika lokální analýza   chemie   MeSH
• antiflogistika analýza   chemie   MeSH
• chromatografie metody   MeSH
• cinchokain analýza   chemie   MeSH
• dexamethason analýza   chemie   MeSH
• lékové roztoky MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• anestetika lokální MeSH
• antiflogistika MeSH
• cinchokain MeSH
• dexamethason MeSH
• lékové roztoky MeSH

The present review dealing with the use of various electrochemical detection systems in flow methods of analysis of drugs (such as FIA and SIA techniques). The review covers the period of 1988 to 1998 and involves 78 references. The drugs determined are arranged according to the functional groups undergoing electrochemical transformation; for all the analytes data on the detection conditions, detection limits and ranges of quantitation are included. Advantages and drawbacks of amperometric detection of drugs in flow systems are discussed.

• MeSH
• elektrochemie metody   MeSH
• léčivé přípravky analýza   MeSH
• průtoková injekční analýza * metody   MeSH
• Publikační typ
• anglický abstrakt MeSH
• časopisecké články MeSH
• Názvy látek
• léčivé přípravky MeSH

In this contribution, the on-line coupling of solid phase extraction (SPE), based on a restricted-access material (RAM), with sequential injection technique (SIA) for the analysis of biological samples, is described. The SIA-RAM system was tested with a new potential antileucotrienic drug (VUFB-19363 (Quinlukast)) for serum analysis. The method is based on SPE with the novel internal-surface reversed-phase column packing material-alkyl-diol silica (ADS). The supports tolerate direct and repetitive injection of proteinaceous fluids (plasma, serum) and allow reversed-phase partitioning at the internal surface. A column packed with a 25 microm C18 alkyl-diol support was used for direct serum injection. Using a 6-port selection valve and the system of three mobile phases, the polar matrix compounds and metabolites are removed by sequentially aspirated mobile phases with lower content of the organic part (methanol-water (2:98) and following acetonitrile-water (20:80)) to the waste, and then, the analyte enriched on the column is eluted by a strong mobile phase (acetonitrile-methanol-water (40:20:40)) to the UV detector without transfer loss. With the fully automated SIA system, a total analysis time of less than 10 min was achieved. The only off-line sample pre-treatment step required to remove particulate matter was centrifugation. The studies showed a range of linearity (2-40 microg ml(-1)) and a high recovery (93.6-96.8%) of drug from the biological matrix with coefficients of variation (RSD) less than 5.0% (n = 6). This paper introduces a new, simple and robust analytical technique suitable for screening determination and direct analysis of drugs in biological materials.

• MeSH
• antagonisté leukotrienů krev   MeSH
• chinoliny krev   MeSH
• kontaminace léku MeSH
• lidé MeSH
• průtoková injekční analýza metody   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• antagonisté leukotrienů MeSH
• chinoliny MeSH
• VUFB19363 MeSH Prohlížeč

This report introduces a fully automated flow system for drug-dissolution studies based on the coupling of the sequential injection analysis (SIA) technique with a conventional dissolution apparatus. The methodology described was used for monitoring of dissolution profiles of prazosin hydrochloride (PRH) in pharmaceutical formulation. The very sensitive fluorimetric detection of PRH was performed at lambda(ex)=244 nm (lambda(em)>or=389 nm). Under the optimal conditions, the calibration curve was linear over the range 0.02-2.43 mg x l(-1) of PRH with R.S.D. 1.89, 1.23, and 1.80% (n=10) when determining 0.02, 1.22, and 2.43 mg x l(-1) of PRH in standard solutions, respectively. Equation of the calibration curve was calculated giving the following values: F=4.108 c-3.9 (n=6), r=0.9996. Detection limit was calculated 0.007 mg x l(-1) of PRH. The dissolution test of Deprazolin tablets was programmed for 60 min, with a continuous sampling rate of 70 h(-1) under conditions required by USP 26. Results obtained by SIA technique compared well with HPLC standard method.

• MeSH
• prazosin analýza   chemie   normy   MeSH
• průtoková injekční analýza metody   normy   MeSH
• řízení kvality MeSH
• rozpustnost účinky léků   MeSH
• spektrofotometrie ultrafialová metody   normy   MeSH
• tablety MeSH
• vysokoúčinná kapalinová chromatografie metody   normy   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• prazosin MeSH
• tablety MeSH

A PC-controlled sequential injection analysis (SIA) system equipped with a spectrophotometric diode-array detector is used for rapid monitoring and evaluation of antioxidation/radical scavenging activity of biological samples. The automated method is based on the known reaction of stable 2,2'-diphenyl-1-picrylhydrazyl radical (DPPH) with antioxidants in organic or aqueous-organic media resulting in bleaching of DPPH due to its "quenching" by the interaction with the analytes. The decrease of the absorbance of DPPH (compared to blank experiment carried out with water-ethanol 1:1 instead of the test solution) measured at 525 nm is related to concentration of an antioxidant in the test solution. With the optimised SIA procedure it is possible to detect down to micromolar concentrations of model antioxidants such as ascorbic acid, caffeic acid, (+)-catechin, (-)-epicatechin and rutin and to evaluate the concentration of these antioxidants in the micromolar to millimolar range. The sample throughput is 45 h(-1). Thanks to its rapidity and sensitivity, the proposed SIA method is suitable for performing routine screening tests for the presence of various antioxidants in large series of lyophilised herbal or mushroom extracts (the amount of sample needed for the analysis is several milligrams).

• MeSH
• antioxidancia metabolismus   MeSH
• automatizace MeSH
• bifenylové sloučeniny metabolismus   MeSH
• biologické faktory metabolismus   MeSH
• časové faktory MeSH
• hydraziny metabolismus   MeSH
• kalibrace MeSH
• koncentrace vodíkových iontů MeSH
• oxidace-redukce MeSH
• pikráty MeSH
• reprodukovatelnost výsledků MeSH
• rostlinné extrakty metabolismus   MeSH
• scavengery volných radikálů metabolismus   MeSH
• spektrofotometrie metody   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• 1,1-diphenyl-2-picrylhydrazyl MeSH Prohlížeč
• antioxidancia MeSH
• bifenylové sloučeniny MeSH
• biologické faktory MeSH
• hydraziny MeSH
• pikráty MeSH
• rostlinné extrakty MeSH
• scavengery volných radikálů MeSH

In the proposed procedure, the determination of bopindolol using a sequential injection technique (SIA) with spectrophotometric detection at 560 nm is described. The new method of determination is based on the color reaction of the indole group in the molecule of bopindolol with 4-dimethylaminobenzaldehyde (Ehrlich's reagent) in acidic medium with production of a violet water-soluble complex. Due to the kinetic standpoint of reaction, the "stopped flow" technique with mixing coil between the valve and detector was tested and optimized. The proposed SIA system was used for the direct determination of bopindolol in tablets, negative effects of interfering substances (excipients of tablets) were not observed. The selectivity of the proposed method of determination was tested in the presence of seven interfering substances from the group of beta-blockers with good results. The interference effect was observed only in the presence of pindolol. The sample throughput with stopped flow technique was 40 samples per hour. Bopindolol was determined in the linear range from 1 to 10 microg ml(-1), RSD was less than 1% (n=10), with limit of detection (3sigma) 0.1 microg ml(-1) and limit of quantification 0.5 microg ml(-1). Obtained results were compared with conventional HPLC method, both analytical techniques were in good agreement.

• MeSH
• benzaldehydy chemie   MeSH
• beta blokátory analýza   MeSH
• pindolol analogy a deriváty   analýza   MeSH
• průtoková injekční analýza přístrojové vybavení   metody   MeSH
• reprodukovatelnost výsledků MeSH
• spektrofotometrie MeSH
• tablety analýza   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• srovnávací studie MeSH
• Názvy látek
• benzaldehydy MeSH
• beta blokátory MeSH
• bopindolol MeSH Prohlížeč
• p-dimethylaminobenzaldehyde MeSH Prohlížeč
• pindolol MeSH
• tablety MeSH