超临界流体色谱法手性拆分左乙拉西坦及其右旋异构体  

Chiral separation of levetiracetam and R-enantiomer by supercritical fluid chromatography

作　　者：金薇[1] 杨新磊[2] 陆丹[1] 杨永健[1] 

机构地区：[1]上海市食品药品检验所,上海201203 [2]安捷伦科技有限公司,上海200233

出　　处：《药物分析杂志》2013年第5期822-826,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立左乙拉西坦及其右旋异构体的超临界流体色谱手性拆分紫外检测方法。方法:采用Chiralcel OD色谱柱(250 mm×4.6 mm,10μm),以超临界二氧化碳-无水乙醇(88∶12)为流动相,流速为2.0 mL.min-1,背压为15 MPa,柱温为40℃,于220 nm波长处分离测定左乙拉西坦及其右旋异构体。结果:右旋异构体与左乙拉西坦依次出峰,分离度为3.7;左乙拉西坦及右旋异构体浓度分别在0.002～0.041 mg.mL-1范围内线性关系良好,相关系数分别为0.9995和0.9994(n=7);定量限分别为34和36 ng(S/N=10),检测限均为10 ng(S/N=3)。结论:超临界流体色谱作为一种绿色环保的色谱方法,分离效率高,重现性好,可有效用于左乙拉西坦及其制剂中右旋异构体的测定及质量控制。Objective：To establish an isocratic supercritical fluid chromatography method for the separation of levetiracetam and its R - enantiomer. Methods： With a Chiralcel OD column （250 mm×4.6 mm,10μm） , well - de-fined separation of levetiracetam and its R - enantiomer was achieved with a mobile phase composed of supercritical C02 with 12% （v/v） anhydrous ethanol as the modifier. The experimental temperature was 40 ℃, back pressure was15 MPa,and the flow rate was 2.0 mL·min^-1 ,with the detection wavelength set at 220 nm. Results： The R -enantiomer and levetiracetam reached peaks successively, with a separation degree of 3.7. Good linear relationshipswere established within the concentration range of 0. 002 -0. 041 mg·mL^-1 for levetiracetam and its R -enantiomer（r =0. 9995 and 0. 9994 ,respectively ,n =7） ,and the quantitative limits（ S/N= 10） were 34 ng and 36 ng,and the detection limits（S/N = 3） were 10 ng and 10 ng,respectively. Conclusion： The proposed method shows high sensitivity, repeatability and stability. It can be employed for the quality control and determination of levetirace-tam and its R -enantiomer.

关 键 词：手性药物质量控制 左乙拉西坦 右旋异构体 超临界流体色谱 二极管阵列检测 手性拆分 

分 类 号：R917[医药卫生—药物分析学]