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柱前衍生化法测定莫西沙星小环的对映异构体 被引量:1

Separation of 2,8-Diazabicyclo Nonane by RP-HPLC after Pre-column Derivatization
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摘要 目的建立柱前衍生化法测定莫西沙星小环对映异构体的方法。方法采用Symmetry C18(4.6mm×250mm,5μm)色谱柱,流动相为甲醇-水(60:40),柱温为35℃;衍生试剂为2,3,4,6.四乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯,检测波长为252nm。结果莫西沙星小环对映体衍生物获得了基线分离,并确认了R,R-衍生物的色谱峰;浓度1.44~72mg/L范围内与峰面积呈线性关系,回归方程为A=34801C-6472(r=0.9999)。结论所建方法简便、快速,可用于莫西沙星小环对映异构体的拆分。 Objective To establish a new RP-HPLC spectrometric method for enantioseparation of 2,8-diazabicyclo[4.3.0] nonane. Methods A Symmetry C18 column (250 mm × 4.6 mm, 5 μm) with a binary solvent mixture of methanol and water (60:40) as the optimized mobile phase was adopted. The separation of enantiomer was studied using 2,3,4,6-tetra-O-acetyl-fl-D-glycopyranosyl isothiocyanate (GITC) as the pre-column derivatizing reagent. The UV detector was set at 252 nm and the column temperature was set at 35 ℃. Results A baseline separation of the enantiomers was achieved, the calibration curve was linear at the range of 1.44-72 mg/L for chlorogenic acid and the equation was A=34 801 C-6472 (r=0.9999). Conclusion The proposed method is feasible, rapid, reliable and can be used for enantioseparation of 2,8-diazabicyclo[4.3.0] nonane.
出处 《食品与药品》 CAS 2013年第3期185-186,共2页 Food and Drug
关键词 吡喃葡萄糖基异硫氰酸酯 莫西沙星小环 反相高效液相色谱法 对映体拆分 柱前衍生化 glycopyranosyl isothiocyanate 2,8-diazabicyclo[4.3.0] nonane RP-HPLC enantioseparation precolumn derivatization
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