Rapid chiral separation and impurity determination of levofloxacin by ligand-exchange chromatography.
Rapid chiral separation and impurity determination of levofloxacin by ligand-exchange chromatography.
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DOI：
10.1016/j.aca.2006.11.023
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发表时间：
2007-02
影响因子：
6.2
通讯作者：
Hongyuan Yan;K. Row
中科院分区：
文献类型：
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作者：
Hongyuan Yan;K. Row
建立了一种灵敏、简单、准确的左氧氟沙星及其(R)-对映体测定方法，采用配体交换高效液相色谱法测定可乐维片材料中左氧氟沙星的手性杂质。研究并评价了不同配体种类、流动相中配体浓度、有机改性剂、流动相pH值和温度对对映体分离的影响。手性分离在常规C18柱上进行，流动相为甲醇-水溶液（含10mmolL−1l-亮氨酸和5mmolL−1硫酸铜）（88:12，v/v），流速设置为1.0mLmin−1。传统的 C18 色谱柱可在 20 分钟内实现两种对映体的基线分离，分辨率为 2.4。通过 Van’t Hoff 图获得的热力学数据（ΔΔH 和 ΔΔS）表明手性分离是一个焓控制的过程。左氧氟沙星及其 (R)-对映体的标准曲线在 0.5 至 400mgL−1 的浓度范围内显示出良好的线性。线性相关方程分别为：y=1.33×105x+6297（r=0.9991）和y=1.34×105x+3565（r=0.9997）。该方法的相对标准偏差（RSD）低于2.3%（n=3）。
A sensitive, simple, and accurate method for determination of levofloxacin and its (R)-enantiomer was developed to determine the chiral impurity of levofloxacin in Cravit Tablets material by ligand-exchange high performance liquid chromatography. The effects of different kinds of ligands, concentration of ligands in mobile phase, organic modifier, pH of mobile phase, and temperature on enantioseparation were investigated and evaluated. Chiral separation was performed on a conventional C18column, where the mobile phase consisted of a methanol–water solution (containing10mmolL−1l-leucine and 5mmolL−1copper sulfate) (88:12, v/v) and its flow-rate was set at 1.0mLmin−1. The conventional C18column offers baseline separation of two enantiomers with a resolution of 2.4 in less than 20min. Thermodynamic data (ΔΔH and ΔΔS) obtained by Van’t Hoff plots revealed the chiral separation is an enthalpy-controlled process. The standard curves showed excellent linearity over the concentration range from 0.5 to 400mgL−1for levofloxacin and its (R)-enantiomer. The linear correlation equations are: y=1.33×105x+6297 (r=0.9991) and y=1.34×105x+3565 (r=0.9997), respectively. The relative standard deviation (RSD) of the method was below 2.3% (n=3).