气相色谱法测定氟西汀残留有机溶剂含量  

Determination of Residual Solvents in Fluoxetine by Gas Chromatography

作　　者：刘秀英[1] 陈建征[1] 郑世君[1] 

机构地区：[1]江苏恩华药业股份有限公司技术中心,江苏徐州221007

出　　处：《福建分析测试》2013年第1期26-28,共3页Fujian Analysis & Testing

摘　　要：目的:建立氟西汀中乙醇、乙醚、正己烷、乙酸乙酯和甲苯残留量的测定方法。方法:采用DB-624毛细管色谱柱(30m×0.53mm,3.0μm),用二甲基亚砜作为溶剂,载气为氮气(0.03MPa),氢火焰离子化检测器(FID),检测器温度240℃;柱温为程序升温;进样口温度150℃;分流比:1:20;进样量1μL。结果:乙醇、乙醚、正己烷、乙酸乙酯和甲苯的线性范围分别为37.89～947.16μg.mL-1(r=0.9999)、39.96～998.90μg.mL-1(r=0.9999)、1.32～32.97μg.mL-1(r=0.9999)、36.02～900.50μg.mL-(1r=0.9996)、6.93～173.20μg.mL-(1r=0.9999),平均回收率(n=9)分别为99.7%、98.5%、100.2%、97.9%和98.6%。结论:该方法操作简单,灵敏度高,结果准确,是测定氟西汀原料中有机残留溶剂的可靠方法。Objective： To establish a Gas chromatography method for the determination of residual ethanol, aether ,n-hexane, ethyl acetate, toluene in Fluoxetine .Methods： DB-624 colmnn （30m × 0.53mm, 3.0 μm ）was adopted, with d imethyl sulfoxide as solvent ,with nitrogen as a carrier gas （0.03MPa） and FID as a detector .the detector temperature was 240℃ ,the column temperature was programmed set;The injecting porl temperatures was 200℃, Injection volume was 1μL and the split ratio was 1：20. Results： ethanol,aether,n-hexane, ethyl acetate,toluene showed a good linear relationship in the range of 37.89 947.16 μg·mL-1（r=0.9999）, 39.96 - 998.90 μg·mL^-1 （r=0.9999）, 1.32 - 32.97μg·mL^-1（r=0.9999） ,36.02 - 900.50 μg·mL-1（r=0.9996） ,6.93-173.20 μg·mL^-1（r=0.9999）,the average recoveries （n=9） of ethanol, aether, n-hexane, ethyl acetate, toluene were 99.7% ,98.5%, 100.2% ,97.9%g198.6% o Conclusion： Gas chromatography （GC） is simple, accurate, sensitive, This is a reliable method to measure residual organic solvents in Fluoxetine.

关 键 词：氟西汀 有机溶剂残留量 气相色谱法 

分 类 号：O657.71[理学—分析化学]