TY - JOUR
T1 - Separation and characterization of a new isomeric impurity in cefalotin sodium by HPLC and MEKC
AU - Yang, Meicheng
AU - Liu, Hao
AU - Qiu, Ya
AU - Wang, Xin
AU - Zhang, Wen
N1 - Publisher Copyright:
© 2015 Taylor & Francis Group, LLC.
PY - 2015/4/21
Y1 - 2015/4/21
N2 - A micellar electrokinetic chromatography (MEKC) method was developed for the determination of impurities in cefalotin sodium. The optimized separation is performed with the background electrolyte composed of 25 mM sodium tetraborate buffer (pH 9.2) containing 0.2 M sodium dodecylsulfate and an applied voltage of 30 kV in a bare fused-silica capillary (50 m i.d. × 64.5 cm, 56 cm detection length). The method was validated in terms of linearity, accuracy, precision, robustness, limit of detection, and limit of quantification. Analyzing the commercial cefalotin sodium and cefalotin sodium CRS with the novel MEKC method, a new impurity was detected in the range of 0.67-1.48% level along with the potential known impurities, which was co-eluted with the main product in the pharmacopoeia high-performance liquid chromatography systems. The new impurity was confirmed to be 3-positional isomer of cefalotin by synthesis, 1H-NMR spectrometry, and MEKC techniques.
AB - A micellar electrokinetic chromatography (MEKC) method was developed for the determination of impurities in cefalotin sodium. The optimized separation is performed with the background electrolyte composed of 25 mM sodium tetraborate buffer (pH 9.2) containing 0.2 M sodium dodecylsulfate and an applied voltage of 30 kV in a bare fused-silica capillary (50 m i.d. × 64.5 cm, 56 cm detection length). The method was validated in terms of linearity, accuracy, precision, robustness, limit of detection, and limit of quantification. Analyzing the commercial cefalotin sodium and cefalotin sodium CRS with the novel MEKC method, a new impurity was detected in the range of 0.67-1.48% level along with the potential known impurities, which was co-eluted with the main product in the pharmacopoeia high-performance liquid chromatography systems. The new impurity was confirmed to be 3-positional isomer of cefalotin by synthesis, 1H-NMR spectrometry, and MEKC techniques.
KW - 3-positionalisomerofcefalotin
KW - H-NMR
KW - cefalotin
KW - HPLC
KW - MEKC
KW - synthesis
UR - https://www.scopus.com/pages/publications/84922111504
U2 - 10.1080/10826076.2014.976709
DO - 10.1080/10826076.2014.976709
M3 - 文章
AN - SCOPUS:84922111504
SN - 1082-6076
VL - 38
SP - 816
EP - 822
JO - Journal of Liquid Chromatography and Related Technologies
JF - Journal of Liquid Chromatography and Related Technologies
IS - 7
ER -