Cemil AYDOĞAN, Veyis KARAKOÇ, Fatma YILMAZ, Huma SHAİKH, Adil DENİZLİ

L-histidin modifiye nanopartiküllerin kiral ligand olarak kullanılması ve ligand değişim kapiler elektroforez yöntemi ile ofloksasinin enantiyoayrılması

L -histidin modifiye nanopartiküllerin kiral ligand ve Cu2+’nin merkez iyon olarak kullanılması ile yeni bir kiral ligand değişim kapiler elektroforez yöntemi geliştirildi. İlk olarak, MAH ve EDMA’nın polimerizasyonu ile polimerik nanopartiküller hazırlandı. Nanopartiküller atomik kuvvet mikroskobu AFM , FTIR ve elemental analiz ile karakterize edildi. Nanopartiküllerin elementel analizi sonucu polimerde 0.2 mmol/g azot olduğu bulundu. Elektrolit çözeltisi içerisinde nanopartiküller içeren kapiler elektroforez sistemi yalancı kapiler elektrokromatografi yöntemi olarak bilinir. Bu yaklaşım ile ofloksasinin enantiyoayırımı, ligand değişim kapiler elektroforez ile yapıldı. Kiral grup içeren nanopartiküller farklı şekilde ofloksasinin yapısal enantiomerleri ile etkileşim gösterdi. Kiral ayırmayı etkileyen faktörler incelendi. Ofloksasin için enantiyoayırma koşulları %70 ACN, 10 mM CuSO4, 40 mM NH4 2SO4 pH 4.7 ve 30 mg/mL nanopartikül olarak optimize edildi. Bu yöntem ile ofloksasinin enantiyoayrılması gerçekleştirildi ve ofloksasin tabletleri ile uygulması yapıldı

Anahtar Kelimeler:

Ligand değişimi, Kapiler elektroforez, ofloksasin, polimerik nanopartiküller

Enantioseparation of Ofloxacin by Ligand Exchange Capillary Electrophoresis Using L-Histidine Modified Nanoparticles as Chiral Ligand

Anovel application of chiral ligand-exchange capillary electrophoresis LE-CE was developed with polymeric nanoparticles as a chiral ligand and Cu 2+ as a central ion. Nanoparticles NPs were prepared by polymerization of N-methacryloyl-L-histidine methyl ester MAH and ethylene dimethacrylate EDMA . NPs were characterized by elemental analysis, fourier transform infrared spectroscopy FTIR , atomic force microscopy AFM . Average particle size and size distribution of NPs were also performed. Elemental analysis of MAH for nitrogen stoichiometry was found as 0.2 mmol/g polymer. CE systems that contain NPs in running buffer can be thought as pseudocapillary electrochromatography. Using this approach, enantiomer separation of ofloxacin was carried out by using LE-CE. The results demonstrated that NPs with chiral functionalized group interacted differently with structural enantiomers of ofloxacin. Factors affecting chiral resolution were studied. The optimum running conditions for the enantioseparation of ofloxacin were found to be a background electrolyte BGE pH 4.7 containing 70% ACN, 10 mM CuSO4, 40 mM NH4 2SO4 and 30 mg/mL NPs. Under these conditions, the enantioseparation of ofloxacin was successfully achieved. With this system, R-ofloxacin and S-ofloxacin levofloxacin were used to analysis capsules in the ofloxacin tablets.

Keywords:

Ligand exchange, Capillary electrophoresis, ofloxacin, polymeric nanoparticles,

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