超临界流体色谱法手性拆分左乙拉西坦及其右旋异构体

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,10 μm),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 uid chromatography method for the separation of levetiracetam and its R-enantiomer. Methods: With a Chiralcel OD column(250 mm×4.6 mm,10 μm),well-defined separation of levetiracetam and its R-enantiomer was achieved with a mobile phase composed of supercritical CO₂ with 12%(v/v) anhydrous ethanol as the modier.The experimental temperature was 40 ℃,back pressure was 15 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 relationships were 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 levetiracetam and its R-enantiomer.

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