Sequential injection analysis
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Tento přehled se zabývá využitím různých elektrochemických detekčních systémů v průtokovýchmetodách analýzy léčiv (jako jsou metody FIA a SIA). Přehled pokrývá období od roku 1988-1998a zahrnuje 78 odkazů. Stanovované léčivé látky jsou seřazeny podle funkčních skupin podléhajícíchelektrochemické transformaci; analytická data zahrnují detekční podmínky, detekční limity a rozsahy kvantity. Rovněž se zabývá výhodami a nevýhodami amperometrické detekce léčiv v průtokových systémech.
The present review dealing with the use of various electrochemical detection systems in flowmethods of analysis of drugs (such as FIA and SIA techniques). The review covers the period of 1988to 1998 and involves 78 references. The drugs determined are arranged according to the functionalgroups undergoing electrochemical transformation; for all the analytes data on the detectionconditions, detection limits and ranges of quantitation are included. Advantages and drawbacks ofamperometric detection of drugs in flow systems are discussed.
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.
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 metody přístrojové vybavení MeSH
- financování organizované MeSH
- lékové formy MeSH
- lidé MeSH
- průtoková injekční analýza metody přístrojové vybavení MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- přehledy MeSH
A proof of concept of a novel pervaporation sequential injection (PSI) analysis method for automatic non-chromatographic speciation analysis of inorganic arsenic in complex aqueous samples is presented. The method is based on hydride generation of arsine followed by its on-line pervaporation-based membrane separation and CCD spectrophotometric detection. The concentrations of arsenite (As(III)) and arsenate (As(V)) are determined sequentially in a single sample zone. The leading section of the sample zone merges with a citric acid/citrate buffer solution (pH 4.5) for the selective reduction of As(III) to arsine while the trailing section of the sample zone merges with hydrochloric acid solution to allow the reduction of both As(III) and As(V) to arsine at pH lower than 1. Virtually identical analytical sensitivity is obtained for both As(III) and As(V) at this high acidity. The flow analyzer also accommodates in-line pH detector for monitoring of the acidity throughout the sample zone prior to hydride generation. Under optimal conditions the proposed PSI method is characterized by a limit of detection, linear calibration range and repeatability for As(III) of 22 μg L(-1) (3sblank level criterion), 50-1000 μg L(-1) and 3.0% at the 500 μg L(-1) level and for As(V) of 51 μg L(-1), 100-2000 μg L(-1) and 2.6% at the 500 μg L(-1) level, respectively. The method was validated with mixed As(III)/As(V) standard aqueous solutions and successfully applied to the determination of As(III) and As(V) in river water samples with elevated content of dissolved organic carbon and suspended particulate matter with no prior sample pretreatment. Excellent relative recoveries ranging from 98% to 104% were obtained for both As(III) and As(V).
- MeSH
- arseničnany izolace a purifikace MeSH
- arsenikové přípravky chemie MeSH
- arsenitany izolace a purifikace MeSH
- chemické látky znečišťující vodu izolace a purifikace MeSH
- kalibrace MeSH
- koncentrace vodíkových iontů MeSH
- kyselina citronová chemie MeSH
- limita detekce MeSH
- průtoková injekční analýza metody MeSH
- řeky chemie MeSH
- spektrofotometrie přístrojové vybavení metody MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
A fully automated sequential injection system was tested in terms of its application in liberation testing, and capabilities and limitations were discussed for clotrimazole liberation from three semisolid formulations. An evaluation based on kinetic profiles obtained in short and longer sampling intervals and steady-state flux values were applied as traditional methods. The obtained clotrimazole liberation profile was faster in the case of Delcore and slower for Clotrimazol AL and Canesten cream commercial formulations. The steady-state flux values for the tested formulations were 52 µg cm-2 h-1 for Canesten, 35 µg cm-2 h-1 for Clotrimazol AL, and 7.2 µg cm-2 h-1 for Delcore measured in 4 min sampling intervals. A simplified approach for the evaluation of the initial rate based on the gradient between the second and third sampling points was used for the first time and was found to correspond well with the results of the conventional methods. A comparison based on the ratio of the steady-state flux and the initial rate values for Canesten and Clotrimazol AL proved the similarity of the obtained results. The proposed alternative was successfully implemented for the comparison of short-term kinetic profiles. Consequently, a faster and simpler approach for dissolution/liberation testing can be used.
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
- financování organizované MeSH
- indomethacin analýza chemie MeSH
- kalibrace MeSH
- lékové formy MeSH
- luminiscenční měření metody přístrojové vybavení MeSH
- molekulární struktura MeSH
- organokovové sloučeniny MeSH
- průtoková injekční analýza metody přístrojové vybavení MeSH
- reprodukovatelnost výsledků MeSH
- rozpouštědla MeSH
- MeSH
- finanční podpora výzkumu jako téma MeSH
- prazosin analýza chemie normy MeSH
- průtoková injekční analýza metody normy MeSH
- řízení kvality MeSH
- rozpustnost MeSH
- spektrofotometrie ultrafialová metody normy MeSH
- tablety MeSH
- techniky in vitro MeSH
- vysokoúčinná kapalinová chromatografie metody normy MeSH