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

作　　者：尹燕杰[1] 何志一[1] 孙超[1] 

机构地区：[1]哈尔滨市食品药品检验检测中心,哈尔滨150525

出　　处：《药物分析杂志》2014年第5期885-888,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：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.

关 键 词：左奥硝唑 右旋异构体 杂质检测 手性分离 手性固定相 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]