顶空气相色谱法测定左乙拉西坦中有机溶剂残留量  

Determination of residual organic solvents in levetiracetam by headspace gas chromatography

作　　者：胡慧廉[1] 丁乃立[1] 吴莲珍[1] 

机构地区：[1]华东理工大学分析测试中心,上海200237

出　　处：《中国新药杂志》2007年第22期1882-1884,共3页Chinese Journal of New Drugs

摘　　要：目的：建立左乙拉西坦中有机溶剂残留量的顶空气相色谱分析方法。方法：选用大口径HP一快速GC残留溶剂柱为分离柱，FID检测器，外标法进行定量，并对分离条件、顶空平衡温度、平衡时间对残留有机溶剂测定的影响进行了研究。结果：二氯甲烷、乙酸乙酯、甲苯的线性范围分别为0．133～1．326μg·mL^-1（r=0．9997），4．330～43．296μg·mL^-1（r=1．0000），0．009～0．087μg·mL^-1（r=0．9997）；平均回收率范围99．70％-102．46％，精密度RSD（n=6）为1．79％-3．05％；检测限分别为0．008，0．005，0．001μg·mL^-1。结论：该方法快速、灵敏、准确。Objective：To establish a method for the determination of three kinds of residual organic solvents in levetiracetam by headspace gas chromatography. Methods：A wide bore HP-fast GC residual solvent column was chosen for separation with FID detector. The external standard method was used for quantitative analysis. Several factors affecting the headspace determination were studied, including analytical conditions, equilibrium temperature and equilibrium time. Results：The standard curves were linear in the range of 0. 133 - 1. 326μg· mL^ - 1 （ r = 0. 999 7） for dichloromethane, 4. 330 ~ 43. 296 μg· mL^ -1 （ r = 1. 000 0 ） for ethyl acetate and 0. 009 - 0. 087μg·mL^ - 1 （ r = 0. 999 7） for toluene. The average recoveries for three residual organic solvents were between 99.70% and 102.46% with RSD （n = 6） of precision in the range of 1.79% -3.05%. The detection limits of dichloromethane, ethyl acetate and toluene were 0. 008,0. 005 and 0. 001μg· mL^-1 respectively. Conclusion ：The method is rapid, sensitive and accurate.

关 键 词：顶空气相色谱法 抗癫痫药物 左乙拉西坦 有机溶剂残留量 

分 类 号：R927.2[医药卫生—药学] R971.9