Improved reversed phase liquid chromatographic method with pulsed electrochemical detection for tobramycin in bulk and pharmaceutical formulation  

作　　者：Vicky Manyanga Ehab Elkady Jos Hoogmartens Erwin Adams 

机构地区：[1]Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, KU Leuven,O&N2, PB 923, Herestraat 49, B-3000 Leuven, Belgium [2]Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St.,Cairo 11562, Egypt

出　　处：《Journal of Pharmaceutical Analysis》2013年第3期161-167,共7页药物分析学报（英文版）

摘　　要：Tobramycin is one of the aminoglycoside antibiotics that lack a UV absorbing chromophore. However, the application of pulsed electrochemical detection （PED） has been used successfully for the analysis of this and similar antibiotics. This work describes an improved liquid chromatographic （LC） method combined with PED, which is able to separate much more impurities than before. Using a Discovery C-18 RP column （250 mm × 4.6 mm i.d., 5 μm）, isocratic elution was carried out with a mobile phase, containing sodium sulfate （35 g/L）, sodium octanesulphonic acid （1 g/L）, tetrahydrofuran （14mL/L） and 0.2 M phosphate buffer pH 3.0 （50 mL/L）. Using these experimental conditions, the limit of quantification （LOQ, S/N= 10） was 5 ng. The linearity was examined in the range LOQ-60 μg/mL and the coefficient of determination was 0.998. The method also proved to be repeatable and the recovery was close to 100%. The influence of the different chromatographic parameters on the separation was investigated by means of an experimental design. The proposed method is useful in quality control of tobramycin drug substances and drug products.Tobramycin is one of the aminoglycoside antibiotics that lack a UV absorbing chromophore. However, the application of pulsed electrochemical detection （PED） has been used successfully for the analysis of this and similar antibiotics. This work describes an improved liquid chromatographic （LC） method combined with PED, which is able to separate much more impurities than before. Using a Discovery C-18 RP column （250 mm × 4.6 mm i.d., 5 μm）, isocratic elution was carried out with a mobile phase, containing sodium sulfate （35 g/L）, sodium octanesulphonic acid （1 g/L）, tetrahydrofuran （14mL/L） and 0.2 M phosphate buffer pH 3.0 （50 mL/L）. Using these experimental conditions, the limit of quantification （LOQ, S/N= 10） was 5 ng. The linearity was examined in the range LOQ-60 μg/mL and the coefficient of determination was 0.998. The method also proved to be repeatable and the recovery was close to 100%. The influence of the different chromatographic parameters on the separation was investigated by means of an experimental design. The proposed method is useful in quality control of tobramycin drug substances and drug products.

关 键 词：Liquidchromatography-Pulsed electrochemicaldetection TOBRAMYCIN Aminoglycosideantibiotics 

分 类 号：R914[医药卫生—药物化学]