A simple and effective high-performance liquid chromatography with ultraviolet detection（HPLC-UV） method was established to determine entecavir optical isomers. With 3 chiral carbon atoms, entecavir had 7 optical is...A simple and effective high-performance liquid chromatography with ultraviolet detection（HPLC-UV） method was established to determine entecavir optical isomers. With 3 chiral carbon atoms, entecavir had 7 optical isomers, including 6 diastereoisomers and 1 enantiomer. The separations were performed on a Symmetrix ODS-AQ C_（18） column（4.6 mm×250 mm, 5 μm） and a Daicel CHIRALPAK AD column（4.6 mm×250 mm, 10 μm）, respectively. The detection wavelength was set at 254 nm. The limit of detection（LOD） and the limit of quantification（LOQ） of diastereoisomers（diastereoisomer-1, diastereoisomer-2, diastereoisomer-3） were 0.0371, 0.0376, 0.0377, and 0.124, 0.125, 0.126 μg/mL, respectively. The LOD and LOQ of enantiomer were 0.14 and 0.46 μg/mL, respectively. The precision was within 0.36%, 0.44%, 1.04%, and 0.67% for diastereoisomer-1, diastereoisomer-2, diastereoisomer-3, and enantiomer, respectively. The recoveries of enantiomers ranged from 98.4% to 100.5%. The method could be applied to control the quality of entecavir.展开更多
基金supported by Chongqing Pharmaceutical Research Institute and Pharmacy School of Chongqing Medical University partly
文摘A simple and effective high-performance liquid chromatography with ultraviolet detection（HPLC-UV） method was established to determine entecavir optical isomers. With 3 chiral carbon atoms, entecavir had 7 optical isomers, including 6 diastereoisomers and 1 enantiomer. The separations were performed on a Symmetrix ODS-AQ C_（18） column（4.6 mm×250 mm, 5 μm） and a Daicel CHIRALPAK AD column（4.6 mm×250 mm, 10 μm）, respectively. The detection wavelength was set at 254 nm. The limit of detection（LOD） and the limit of quantification（LOQ） of diastereoisomers（diastereoisomer-1, diastereoisomer-2, diastereoisomer-3） were 0.0371, 0.0376, 0.0377, and 0.124, 0.125, 0.126 μg/mL, respectively. The LOD and LOQ of enantiomer were 0.14 and 0.46 μg/mL, respectively. The precision was within 0.36%, 0.44%, 1.04%, and 0.67% for diastereoisomer-1, diastereoisomer-2, diastereoisomer-3, and enantiomer, respectively. The recoveries of enantiomers ranged from 98.4% to 100.5%. The method could be applied to control the quality of entecavir.
