毛细管顶空气相色谱法测定左乙拉西坦中的残留溶剂

Determination of residual solvents in levetiracetam by head space gas capillary chromatography

目的建立毛细管顶空气相色谱法测定左乙拉西坦有机残留溶剂。方法选用气相色谱配备顶空进样器法进行测定,DB-624毛细管柱作为分析柱,采用FID检测器;并对溶剂测定有影响的因素进行研究。结果甲醇在12~90μg·mL^(-1)、丙酮在20~150μg·mL^(-1)、二氯甲烷在1.44~10.8μg·mL^(-1)、乙酸乙酯在20~150μg·mL^(-1)与峰面积线性关系良好(r>0.999);各组分检测限分别为0.032、0.021、0.11、0.011μg·mL^(-1);4种溶剂回收率均在90%~110%以内,RSD<10.0%(n=5)。结论该方法简单、可靠、准确,可用于左乙拉西坦有机残留溶剂的测定。

Objective To establish a head space gas capillary chromatography method to determine residual solvents in levetiracetam. Methods Head space gas capillary chromatography, FID detector, and DB-624 capillary column were used. Some factors which affected the determination of residual solvents were studied. Results The calibration curves of solvents had a good linearity at 12 - 90 μg·mL -1 for methanol, 20 - 150 μg·mL -1 for acetone, 1.44 - 10.8μg·mL -1 for dichloromethane, and 20 - 150 μg·mL -1 for ethyl acetate. The correlation cofficient of each content was more than 0.999. The detection limit was 0.032 μg·mL -1 for methanol, 0.021 μg·mL -1 for acetone, 0.11 μg·mL -1 for dichloromethane, and 0.011 μg·mL -1 for ethyl acetate. The recoveries of the 4 solvents were within 90% - 110%, RSD 〈 10% （n = 5）. Conehlsion The method is simple, reliable and accurate for the determination of residual solvents in levetiracetam.