盐酸阿扎司琼有机溶剂残留量测定  

Determination of Organic Volatile Impurities in Azasetron Hydrochloride

作　　者：王彦[1] 

机构地区：[1]上海市药品检验所,上海200233

出　　处：《药物分析杂志》2004年第3期293-295,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立了气相色谱法测定盐酸阿扎司琼合成工艺中用过的1,2-二氯乙烷、氯仿、甲苯、碘甲烷、乙醇与乙醚有机溶剂残留量。方法:气相色谱法,顶空进样,氢火焰离子化检测器(FID),以水为溶剂,采用甲基聚硅氧烷和5%苯基-95%甲基聚硅氧烷毛细管色谱柱串联(HP-1+HP-5:30 m×0.53 mm+10 m×0.53 mm)。进样口温度200℃,检测器温度250℃,顶空取样瓶在90℃加热18 min。柱温先在35℃恒温6 min,然后以每分钟40℃的升温速率升至150℃,维持4 min。结果:各成分线性试验所得回归方程,相关系数均在0.99以上,最低检出限分别为0.3,1.3,18,41.3,13,6.7 ng。加样回收率均在 96.0%-101.5%,RSD<2.O%(n=9)。结论:经方法学试验验证,该方法准确、灵敏、可靠,测得各组分的线性、精密度、加样回收结果良好。Objective: An GC method for determination of 1,2 -dichloroethane, chloroform, toluene, methyl iodine, ethanol and ether in synthetic azasetron hydrochloride was developed. Methods: Head space samples were injected onto GC, using following capillary columns in series HP - 1 (100% dimethylpoly - siloxane 30 m × 0. 53 mm ) and HP-5 (5%diphenyl and 95% dimethylpolysiloxane 10 m ×0. 53 mm ).The intial temperature was kept at 35℃ for 6 min,then the temperature was raised to 150℃ at the rate of 40℃·min-1 ,and subsequently sustained for 4 min. The injection port and detector temperature were 200℃ and 250℃ respectively. Results:The correlation coefficient of the calibration curve of each content in quercetin was >0. 99. The limits of determination were 0.3,1.3, 18,41. 3,13,6. 7 ng respectively. The recoveries were between 96. 0% and 101. 5% ,RSD < 2.0% (n =9). Conclusion: The method was proved to be accurate, sensitive and reliable. The results for linearity,precision and recoveries were good.

关 键 词：盐酸阿扎司琼 有机溶剂 残留量 气相色谱法 

分 类 号：R965[医药卫生—药理学]