摘要
目的:建立以毛细管气相色谱法测定异氟烷中丙酮、N,N-二甲基甲酰胺、N-甲基吡咯烷酮等3种有机溶剂残留量的方法。方法:色谱柱为DB-624石英毛细管柱,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为150℃,以环己烷为溶解介质。结果:丙酮、N,N-二甲基甲酰胺、N-甲基吡咯烷酮的检测浓度的线性范围分别为0.1~5.00(r=0.9999)、0.0176~0.88(r=0.9999)、0.0106~0.53(r=1.0000)mg·mL-1;平均回收率为97.5%~98.7%(RSD=0.4%~0.6%);最低检出限为1.46~4.49ng;3批样品中3种有机溶剂残留量均符合《中国药典》要求。结论:该方法操作简便、精密度好,结果准确可靠,可用于异氟烷中有机溶剂残留量的测定。
OBJECTIVE:To establish a capillary GC method for the determination of residual organic solvents including acetone, N,N-dimethylformamide and N-methyl pyrrolidone in isoflurane.METHODS:The residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃,the inlet temperature was 150 ℃,and cyclohexane as the solvent. RESULTS:The linear ranges of acetone, N,N-dimethylformamide and N-methyl pyrrolidone were 0.1~5.00 (r=0.999 9),0.017 6~0.88 (r=0.999 9),0.010 6~0.53 (r=1.000 0) mg·mL-1 respectively. The average recoveries ranged from 97.5% to 98.7% with RSD ranged at 0.4%~0.6%.The detection limits were 1.46~4.49 ng.The residual levels for the three organic solvents in 3 batches of samples were all up to the standard stipulated in China Pharmacopeia. CONCLUSION:The method is simple,accurate,sensitive and reproducible,it can be used for the determination of the residual organic solvents in isoflurane.
出处
《中国药房》
CAS
CSCD
北大核心
2010年第17期1595-1596,共2页
China Pharmacy
关键词
异氟烷
有机溶剂
残留量
毛细管气相色谱法
Isoflurane
Organic solvents
Residual
Capillary gas chromatography