Grant-funded Project Nr. 264/2003/B-CH/FaF
Final Report

Project title:Using of monolithic columns in the system of sequential injection technique for drug analysis
Research leader:Mgr. Dalibor Šatínský
Co-researcher: Doc.RNDr. Petr Solich, CSc.; Mgr. Jitka Huclová; Mgr. Jana Klimundová
Period of project:2003-2003
Overall grant:134 000 CZK

Project Results

The main solution of the research project was coupling of monolithic columns to the system of sequential injection analysis, pharmaceutical sample preparation, SIA program optimization and to choose available monolith for simple sample separation. The column was placed between the selection valve and flow cell of the detector. The selection valve was used as autosampler for sample preparation and calibration. The above mentioned coupling allows automation and acceleration of simple separation process without need of HPLC instrumentation
SIA separations with the using of new method of Sequential injection chromatography (SIC) were directed to the
development and validation of simple separation methods, which can replace HPLC method with SIC in some special cases. The new developed SIC methods were validated and compared with the same HPLC methods. The good correlation was observed between the both methods.
The three original methods of drug determination in pharmaceutical preparations were carried out during the problem solution. It was determination of salicylic acid and methylsalicylate in antiinflammatory cream preparations (APHLOX paste (Herbacos Bofarma s.r.o)), determination of triamcinolon acetonide and methyl- and propylparabens in antiinflammatory gels (Triamcinolon gel (Herbacos Bofarma s.r.o)). The next method developed was SIC separation and determination of acetylsalicylic acid, caffeine and paracetamol in analgesic-antipyrretic tablets ACIFEIN, ACYLCOFFIN (SLOVAKOFARMA, Hlohovec) and PANADOL EXTRA (SmithKline Becham Consumer Healthcare).
The last SIC method of determination of ambroxol, methylparaben and benzoic acid in pharmaceutical syrups is under construction. The obtained results of methods determination were published in special analytical journals with high impact factors and they were presented on the analytical conferences in Slovakia republic and Greece.
The character of our work was mainly development and experimental. The main task of the project - coupling of SIA with chromatographic procedures is highly original and no published on the analytical field home and abroad. The successful solution of this project was important for our department at the international level. The good results of validation of SIC methods show on the possibility of the method expansion to the future (we have received a number of requests for our reprints from foreign departments).
Published works with GA UK support:1.) Huclová J., Šatínský D., Karlíček R.: Coupling of monolithic columns with sequential injection technique. A  new separation approach in flow methods, Anal. Chim. Acta 494 (2003) 133-140. 2.) Šatínský D., Neto I., Solich P., Montenegro M. C., Araújo A. N.: Sequential injection chromatographic determination of paracetamol, caffeine and acetylsalicylic acid in pharmaceutical tablets, J. Sep. Sci. – in press.
Posters: 1.) Šatínský D., Huclová J., Solich P., Karlíček R.: Reversed-phase porous silica rods: an alternative tool of separation in sequential injection technique, 3rd International Conference of Instrumental Method of Analysis, Soluň, Řecko, 2003 2.) Šatínský D., Huclová J., Solich P., Karlíček R.: Reversed-phase porous silica rods: an alternative approach to HPLC separation using sequential injection chromatography technique, Velké Karlovice, 32. Konference syntéza a analýza léčiv 3.) D. Šatínský, J. Klimundová et. al. - poster in press.