气相色谱法测定硫酸阿扎那韦中残留溶剂的含量  

Determination of Residual Solvents in Azanavir Sulfate by Gas Chromatography-Flame Ionization Detector

作　　者：周洁 高衎 李春刚 唐祁匀 ZHOU Jie;GAO Kan;LI Chun-gang;TANG Qi-yun(Shanghai Shyndec Pharmceutical(Haimen)Co.,Ltd.,Nantong 226100,Jiangsu China)

机构地区：[1]上海现代制药海门有限公司,江苏南通226100

出　　处：《分析测试技术与仪器》2020年第4期282-287,共6页Analysis and Testing Technology and Instruments

摘　　要：采用甲醇-正丁醇(体积比1∶1)为稀释液配制样品,消除乙醇、异丙醇与阿扎那韦形成的溶剂合物,建立了气相色谱测定硫酸阿扎那韦中残留溶剂的方法.试验条件:FID检测器,其温度为240℃;进样口温度200℃,分流比20∶1;载体为氮气,流速1 mL/min;色谱柱初始温度35℃,保持3 min,以2℃/min的升温速率上升到70℃,再以20℃/min的升温速率上升到220℃,维持2 min.试验结果表明空白溶剂及样品不干扰测定,各残留溶剂峰之间分离度良好.乙醇、丙酮、异丙醇、二氯甲烷、甲基叔丁基醚和正庚烷的检测限分别为2.063、0.575、2.001、4.379、0.875、0.504μg/mL,方法专属、灵敏.且上述溶剂分别在5.16~751.23、1.74~722.29、5.00~754.03、13.27~89.79、2.65~750.12、1.53~749.43μg/mL范围内,其质量浓度与峰面积的线性关系良好(r为0.9990~1.0000).方法的RSD均低于5.0%,回收率结果均介于90%~110%之间,方法重复性及准确度较好.可适用于硫酸阿扎那韦中的残留溶剂的测定.A method to determine residual solvent in Azanavir sulfate by gas chromatography(GC)has been set up.And the sample preparation method using methanol:n-butanol(1∶1,V/V)as the diluent was clarified particularly to eliminate the problem of interference in the determination.Test conditions of the flame ionization detector(FID)were as follows:temperature:240℃,temperature of injection port:200℃,split ratio:20∶1,carrier gas:N 2,flow rate:1 mL/min.The initial temperature of the chromatographic column was 35℃,kept for 3 min,then increased to 70℃at a heating rate of 2℃/min,and then increased to 220℃at a heating rate of 20℃/min,and maintained for 2 min.The results showed that the interference problem of solvent mixture was solved,and the blank solution and Azanavir sulfate did not interfere the solvents to be tested,and all the residual solvent peaks were well separated,so the specificity was good.The LODs of ethanol,acetone,isopropanol,dichloromethane,methyl tert-butyl ether,n-heptane were 2.063,0.575,2.001,4.379,0.875,0.504μg/mL respectively.The linearities of above solvents were acceptable in the range of 5.16~751.23,1.74~722.29,5.00~754.03,13.27~89.79,2.65~750.12,1.53~749.43μg/mL(r=0.9990~1.0000)respectively.The RSD of the same homogenous sample was less than 5.0%,so the method was reproducible.The recoveries of all the results were in the range of 90%~110%,so the method was accurate.The method was suitable for testing residual solvents in Azanavir sulfate.

关 键 词：硫酸阿扎那韦 气相色谱法 溶剂合物 

分 类 号：O657.71[理学—分析化学]