论文部分内容阅读
目的利用HPLC法同时测定左乙拉西坦中工艺杂质、降解杂质及中间体。方法采用Kromasil 100-5 C18色谱柱(250 mm×4.6 mm,5μm),以体积分数为0.1%三乙胺水溶液(用磷酸调节p H值至5.5)-乙腈(体积比为9∶1)为流动相,检测波长为205 nm,流速为1.0 m L·min-1,柱温为35℃。结果 8个杂质在考察的质量浓度范围内与峰面积之间呈良好的线性关系(r≥0.999 9);检测限均在7~240μg·L-1内;平均回收率均在99.2%~107.3%内,RSD均小于3.0%(n=9)。结论本方法简便、准确、专属性强、灵敏度高,可用于左乙拉西坦的质量控制。
OBJECTIVE To simultaneously determine the technical impurities, degradation impurities and intermediates of levetiracetam by HPLC. Methods A Kromasil 100-5 C18 column (250 mm × 4.6 mm, 5 μm) was used. The volume fraction of 0.1% triethylamine in water (adjusted to pH 5.5 with phosphoric acid) -acetonitrile (9: 1 by volume) The mobile phase was detected at a wavelength of 205 nm with a flow rate of 1.0 mL · min-1 and a column temperature of 35 ℃. Results The results showed that there was a good linear relationship between the concentration of 8 impurities and the peak area (r≥0.999 9), the detection limits were all within 7 ~ 240 μg · L-1, and the average recoveries were between 99.2% and 107.3 % RSDs were less than 3.0% (n = 9). Conclusion The method is simple, accurate, specific, sensitive and can be used for the quality control of levetiracetam.