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顶空毛细管GC法测定马波沙星原料药中6种溶剂的残留量
董玲玲,汪霞,杨星,马秋冉,于晓辉,赵富华
0
(中国兽医药品监察所)
摘要:
建立顶空毛细管气相色谱法测定马波沙星原料药中甲醇、乙醇、乙腈、二氯甲烷、苯和甲苯等6种溶剂残留量。色谱柱为DB-624毛细管柱(30m×0.53mm,3.0μm),采用程序升温的方式,检测器为火焰离子化检测器(FID),检测器温度为250℃;顶空瓶平衡温度为105℃,平衡时间为20min。结果显示在该色谱条件下,6种溶剂均能得到良好分离; 加样回收率均在100%~110%之间(RSD<8%,n=9),精密度重复性和稳定性结果均良好;该方法操作简便,重复性高,结果稳定可靠,可用于马波沙星残留溶剂的检测。
关键词:  马波沙星  GC  残留溶剂
DOI:
投稿时间:2021-04-25修订日期:2021-11-25
基金项目:
Determination of 6 kinds of residual solvents in Marbofloxacin bulk drug by headspace capillary gas chromatography
(China Institute of Veterinary Drug Control)
Abstract:
A method for the simultaneous determination of six kinds of residual solvents as methanol, ethanol, acetonitrile, dichromethane, benzene and toluene in Marbofloxacin draw material was established by headspace gas chromatography. The residual solvents were seperated on DB-624 (30m×0.53mm, 3.0μm) capillary column using temperature programming. FID was used as detector with the temperature of 250°C. The sample was extracted at105℃for 20min.The results showed that the separation of six kinds of residual solvents was good. The average recoveries were ranged from 100%~110%(RSD<8%,n=9). Results of precision,repeatability and stability were good. Therefore, the established method which is simple,reproducible, stable and reliable can be used for detection of residual solvents in Marboflocaxin draw material.
Key words:  Mabofloxacin  gas chromatography  residual solvents

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