Polipirolün Yüksek Performanslı Sıvı Kromatografide Potansiyometrik Dedektör Olarak Kullanımı

Özet: Bu çalışmada 4 adet sülfonamit grubu bileşiğin (sülfonilamit, sülfodiazin, sülfometazin, sülfomonometoksin) kromatografik davranışları, polipirolün potansiyometrik dedektör olarak kullanıldığı HPLC yöntemi ile incelenmiştir. %15, 30, 40 ve 50 (v/v) asetonitril-su ikili karışımlarında pH 1,5-7,0 aralığında hazırlanan Britton-Robinson tampon çözeltileri kullanılarak asetonitril-su oranı ve pH etkisi belirlenmiştir. Polipirol potansiyometrik dedektör, camsı karbon yüzeyinde pirolün elektropolimerizasyonu ile hazırlanmıştır. Bileşiklerin tayin limitleri sülfonilamit için 1,92.10-6 M; sülfodiazin için 2,12.10-6 M; sülfomerazin için 1,83.10-6 M; sülfomonometoksin için 1,25.10-6 M olarak hesaplanmıştır. Anahtar Kelimeler: Sülfonamit, Polipirol, Potansiyometrik dedektör, HPLC Abstract: In this study, the chromatographic behaviors of four sulfonamides (sulfanilamide, sulfadiazine, sulfamerazine, sulfamonomethoxine) were investigated by a HPLC using polypyrrole as a potentiometric detector. The effect of acetonitrile-water ratio and pH were determined for %15, 30, 40 and 50 (v/v) acetonitrile/water binary mixture between pH 1.5 and 7.0 prepared Britton-Robinson buffers,. The polypyrrole potentiometric detector was prepared by electropolymerization on the surface of glassy carbon. Detection limits of these compounds were calculated as: 1.92.10-6 M for sulfanilamide; 2.12.10-6 M for sulfadiazine; 1.83.10-6 M for sulfamerazine; 1.25.10-6 M for sulfamonomethoxine. Key words: Sulfonamide, Polypyrrole, Potentiometric detector, HPLC

___

  • Chriswanto H., Wallace G.G., 1996. Redox chromatography using polypyrroles a stationary phase, Journal of Liquid Chromatography, 19 (15): 2457-2479.
  • Brambilla G., Fiori M., Rizzo B., Crescenzi V., Macsi G., 2001. Use of molecularly imprinted polymers in the solid-phase extraction of clenbuterol from animal feeds and biological matrices, Journal of Chromatography B, 759 (1): 27-32.
  • Perruchot C., Cheimi M.M., Delamar M., Dardoize F., 2002. Characterization of the chromatographic properties of a silica-polypyrrole composite stationary phase by inverse liquid chromatography, Journal of Chromatography A, 969 (1-2): 167-180.
  • Trojanowicz M., 2003. Application of conducting polymers in chemical analysis, Microchimica Acta, 143 (2-3): 75-91.
  • John R., Ongarato D.M., Wallace G.G., 1996. Development of a conducting polymer-based microelectrode array detection system, Electroanalysis, 8 (7): 623-629.
  • Barisci J.N., Wallace G.G., Clarke A., 1997. Amperometric detection of electroinactive anions using conducting polymer electrodes subsequent to chromatography separation, Electroanalysis, 9 (6): 461-467.
  • Staes E., Vangeneugden D., Nagels N.J., Vanderzande D., Gelan J., 1999. Properties of a low band gap conducting polymer electrode used for amperometric detection in liquid chromatography, Electroanalysis, 11 (1): 65-69.
  • Wang J., Jiang M., Kawde A., 2000. Flow detection of UV radiation-induced DNA damage at a polypyrrole-modified electrode, Electroanalysis, 13 (7): 537-540.
  • Akhtar P., Too C., Wallace G.G., 1997. Detection of haloacetic acids at conductive electroactive polymer-modified microelectrodes, Analytica Chimica Acta, 341 (2-3): 141-153.
  • Xu Q., Wang Y.P., Zhang W., Jing L., Tanaka K., Haraguchi H., Itoh A., 2000. Amperometric detection studies of poly-o-phenylenediamine film for the determination of electroinactive anions in ion-exclusion chromatography, Analyst, 125 (8): 1453-1457.
  • Poels I., Nagels L.J., Verreyt G., Geise H.J., 1998. Potentiometric detection of organic acids in liquid chromatography using conducting oligomer electrodes, Analytica Chimica Acta, 370 (2-3): 105- 113.
  • Şahin M., Şahin Y., Özcan A., 2008. Ion chromatography-potentiometric detection of inorganic anions and cations using polypyrrole and overoxidized polypyrrole electrode, Sensors and Actuators B, 133 (1): 5-14.
  • Cross R.F., Cao J., 1998. Salt effects in capillary zone electrophoresis III. Systematic and selective factors in the high ionic strength separation of sulfonamides in sodium phosphate buffers, Journal of Chromatography A, 818 (2): 217-229.
  • Jen J.F., Lee H.L., Lee B.N.,1998. Simultaneous determination of seven sulfonamides residues in s wine wastewater by high-performance liquid chromatography, Journal of Chromatography A, 793 (2): 378-382.
  • Stoev G., Michailova A., 2000. Quantitative determination of sulfonamide residues in foods of animal origin by high-performance liquid chromatography with fluoresence detection, Journal of Chromatography A, 871 (1-2): 37-42.
  • Hela W., Brandtner M., Widek R., Schuh R., 2003. Determination of sulfonamides in animal tissues using cation exchange reversed phase sorbent for sample cleanup and HPLC-DAD for detection, Food Chemistry, 83 (4): 601-608.
  • Rao T.N., Sarada B.V., Tryk D.A., Fujishima A., 2000. Electroanalytical study of sulfo drugs at diamond electrodes and their determination by HPLC with amperometric detection, Journal of Electroanalytical Chemistry, 491 (1-2): 175-181.
  • Preechaworapun A., Chuanuwatanakul S., Einaga Y., Grudpan K., Motomizu S., Chailapakul O., 2005. Electroanalysis of sulfonamides by flow injection system/high-performance liquid chromatography coupled with amperometric detection using boron-doped diamond electrode, Talanta, 68 (5): 1726-1731.
  • Torres-Lapasio J.R., Garcia-Alvarez-Coque M.C., Bosch E.; Roses M., 2005. Considerations on the modelling and optimisation of resolution of ionisable compounds in extended pH-range columns, Journal of Chromatography A, 1089 (1-2): 170-186.
  • Pingarron Carrazon J.M., Dominguez Recio A., Polo Diez L.M., 1992. Electroanalytical study of sulphamerazine at a glassy-carbon electrode and its determination in pharmaceutical preparations by HPLC with amperometric detection, Talanta, 39 (6): 631-635.
  • Titus A.M., Msagati J., Catherine N., 2002. Voltammetric detection of sulfonamides at a poly(3- methylthiophene) electrode, Talanta, 58 (3): 605-610.
  • Souza C.D., Braga O.C., Vieira I.C., Spinelli A., 2008. Electroanalytical determination of sulfadiazine and sulfamethoxazole in pharmaceuticals using a boron-doped diamond electrode, Sensors and Actuators B: Chemical, 135 (1): 66-73.
  • Braga O.C., Campestrini I., Vieira I.C., Spinelli A., 2010. Sullfadiazine determination in pharmaceuticals by electrochemical reduction on a glassy carbon electrode, Journal of Brazilian Chemical Society, 21 (5): 813-820.
  • Yücel Şahin e-posta: ysahin@anadolu.edu.tr
  • Güleren Alsancak e-posta: gulerenalsancak@sdu.edu.tr