顶空毛细管气相色谱法检测福尔可定中的残留溶剂  

Determination of Residual Solvents in Pholcodine by Headspace Capillary Gas Chromatography

作　　者：李振洲 胡雯 汪汶 张瑞娟 张丽娜 钟凯 田军 Li Zhenzhou;Hu Wen;Wang Wen;Zhang Ruijuan;Zhang Lina;Zhong Kai;Tian Jun(Yichang Humanwell Pharmaceutical Co,LTD,Yichang 443000,China)

机构地区：[1]宜昌人福药业有限责任公司,湖北宜昌443000

出　　处：《巴楚医学》2020年第2期63-66,共4页Bachu Medical Journal

基　　金：国家重大新药创制项目(No:2011ZXJ09302)。

摘　　要：目的:建立顶空毛细管气相色谱法检测福尔可定中甲醇、乙醇、氯乙醇和苯4种有机溶剂的含量。方法:色谱柱为CP7416(6%氢丙基苯基-94%二甲基聚硅氧烷为固定相),载气为氮气,检测器为氢火焰离子检测器,顶空平衡温度为90℃,顶空平衡时间为30 min,检测器温度为250~300℃,进样口温度为150~180℃,柱温为65~75℃。结果:检测柱的耐用性及专属性好;甲醇、乙醇、氯乙醇和苯的检测限分别为7.5 ppm、11.9 ppm、1 ppm、220 ppm;11批样品中4种溶剂的残留结果均符合2015年版《中国药典》的相关要求。结论:本方法操作简单、灵敏度高、准确性好,可用于福尔可定中残留溶剂的质量控制。Objective:To establish headspace capillary gas chromatography for the determination of methanol,ethanol,chlorine ethanol and benzene in Pholodine.Methods:The chromatographic column was CP7416,with 6%hydropropyl phenyl-94%dimethyl polysiloxane as the stationary phase.The carrier gas was nitrogen and the detector was flame ionization detector(FID).The temperature headspace equilibrium was 90℃,and the headspace time was 30 min.The temperature of detector and injector were 250℃to 300℃,and 150℃to 180℃,respectively.The column temperature was 65℃to 75℃.Results:The test column had good durability and specificity.The limit of detection for methanol,ethanol,chlorine ethanol and benzene were 7.5 ppm,11.9 ppm,1 ppm and 220 ppm,respectively.Residual solvent results of 4 solvents in 11 batches of samples were in line with the requirements of Chinese Pharmacopoeia(2015 edition).Conclusion:Headspace capillary gas chromatography is simple,sensitive and accurate,which can be used for the quality control of the residual solvents in Pholcodine.

关 键 词：顶空气相色谱法 福尔可定 残留溶剂 

分 类 号：R927.11[医药卫生—药学]