摘要
为了建立测定加米霉素原料药中甲醇、乙醇、正丙醛、二氯甲烷与正庚烷5种溶剂残留量,本试验建立一种基于顶空气相色谱法的检测方法:色谱柱为DB-624石英毛细管柱(30.0 m×0.53 mm,3μm);氢火焰离子化检测器,温度为250℃;程序升温;载气为氮气,流速为2.5 mL/min;顶空平衡温度为70℃,平衡时间10 min。结果显示,甲醇、乙醇、正丙醛、二氯甲烷与正庚烷在各自的浓度范围内均线性关系良好,检测限分别为0.599、1.008、0.352、0.301μg/mL和0.030μg/mL,平均回收率为98.9%~103.8%。结果表明该方法可用于加米霉素原料药的残留溶剂测定。
The aim of the study was to establish a method for determination of five residual solvents in gamithromycin source material.The headspace gas chromatography was performed on a capillary column DB-624(30.0 m×0.53 mm,3 μm) with programmed temperature.An FID detector was used with a temperature of 250 ℃.The carrier was nitrogen with a flow rate of 2.5 mL/min.The headspace equilibrium temperature and time duration was respectively set at 70 ℃ and 10 min.The results showed that the linear relationships of methanol,ethanol,n-propanal,dichloromethane and n-heptane were very well in respective concentration ranges,and the average recovery was 98.9%-103.8%;and that the limits of detection were 0.599,1.008,0.352,0.301 μg/mL and 0.030 μg/mL,respectively.Thus,the method described in this study would meet the requirements of residual solvents detection in gamithromycin source material.
作者
岳永波
范小平
李伟岭
杨芳
刘波
吴鹏飞
罗妍
赵盼
王金阳
YUE Yong-bo;FAN Xiao-ping;LI Wei-ling;YANG Fang;LIU Bo;WU Peng-fei;LUO Yan;ZHAO Pan;WANG Jin-yang(Baoding Jizhong Pharmaceutical Co.Ltd.,Baoding 071500,China;Shijiazhuang Jizhong Pharmaceutical Co.Ltd.,Shijiazhuang 050066,China;Hainan Animal Disease Prevention and Control Center,Haikou 571100,China)
出处
《中国兽医杂志》
CAS
北大核心
2021年第10期48-51,共4页
Chinese Journal of Veterinary Medicine
关键词
加米霉素
顶空进样
气相色谱
残留溶剂
gamithromycin
headspace sampling
gas chromatography
residual solvents