高效液相色谱法分离和测定左奥硝唑中右旋异构体

HPLC separation and determination of dextroisomer in levornidazole

目的：建立手性高效液相色谱方法,用于测定左奥硝唑原料和制剂中的右旋异构体。方法：采用CHIRALPAK IC（250 mm×4.6 mm,5μm）手性柱,以正己烷-无水乙醇（90∶10）为流动相,流速1.0 mL·min-1,检测波长308 nm。结果：奥硝唑对映体之间的分离度为3.9,奥硝唑右旋异构体的检测限为0.52 ng;线性范围为1.05～21.0μg·mL-1;低、中、高浓度的回收率（n=3）分别为101.3%、100.2%、100.5%,RSD分别为1.3%、0.9%、1.5%;供试溶液在12 h内基本稳定;温度和流速的影响试验表明该方法有良好的耐用性。结论：所建立的方法经方法验证可用于分离和测定左奥硝唑原料和制剂中的右旋异构体杂质。

Objective： To develop an HPLC method for the separation and determination of the dextroisomer in raw materials and preparations of levornidazole. Methods： The separation was performed on the CHIRALPAK IC（ column 250 mm × 4. 6 mm,5 μm） with the mobile phase of hexane-alcohol（ 90∶ 10） at a flow rate of 1. 0 mL· min-1,and the detective wavelength was set at 308 nm. Results： The resolution between the peaks of levornidazole and its enantiomer was 3. 9; the detection limit of dextroisomer was 0. 52 ng. The linear range was 1. 05-21. 0 μg· mL-1; the recovery（ n =3） at low,medium and high concentrations was 101. 3%,100. 2%,100. 5%; RSD was 1. 3%, 0. 9%,1. 5%,respectively. The test solution was basically stable within 12 h. The influence test of temperature and speed showed that the method had good durability. Conclusion： The method is quick and accurate,and suitable for separation and determination of dextroisomer impurity in raw materials and preparations of levornidazole.