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顶空气相色谱法测定阿德福韦酯中4种有机溶剂残留量 被引量:3

Determination of four residual organic volatile solvents in adefovir dipivoxil by head space-gas chromatography
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摘要 目的:测定阿德福韦酯中有机溶剂乙腈、二氯甲烷、异丙醚和甲苯的残留量。方法:采用顶空进样法,氢焰离子化检测器(FID),以稀盐酸为溶剂,采用不锈钢填充柱(2m×3mm),以二乙烯苯与乙基乙烯苯高分子多孔小球(粒径0.25~0.18mm)为填充材料,柱温:180℃;氢火焰检测器温度:200℃;载气:氮气;载气流速:50mL.min-1。结果:实现了4个组份的基线分离,乙腈、二氯甲烷、异丙醚、甲苯4种有机溶剂分别在0.40~3.2,0.60~4.8,1.0~8.0,0.80~6.4μg.mL-1浓度范围内呈现良好线性,线性相关系数分别为0.9989,0.9994,0.9989,0.9990。回收率分别为96.7%,98.2%,96.9%和96.1%。检出限分别小于0.40,0.20,0.20和0.08μg.mL-1。3批样品中4种有机溶剂残留量均符合要求。结论:该方法简单,灵敏,准确度高,适用于阿德福韦酯中有机溶剂残留量的控制。 s Objective:To determine the contents of residual volatile organic solvents acetonitrile,dichloromethane,iso-prop ether and toluene in adefovir dipivoxil.Methods:Using head space-GC method,sample was dissolved in HCl aqueous solution(9→1 000)which had been equilibrated at 60℃ for 60 minutes.A stainless steel column(2 m×3 mm)packed with ethylvinylbenzene-divinyl benzene copolymer(diameter from 0.25~0.18 mm)was used at 180℃.The injection port and detector temperature was 200℃ respectively.Using nitrogen as the carrier gas at flow rate of 50 mL·min-1.Under the above conditions,the volatile organic solvents were separated completely.Results:The method proved to be linear in the ranges of 0.40~3.2,0.60~4.8,1.0~8.0,0.80~6.4 μg·mL-1 and the average recovery was 96.7%,98.2%,96.9%,96.1% for acetonitrile,dichloromethane,iso-prop ether and toluene respectively.The detection limit was less than 0.40,0.20,0.20,0.08 μg·mL-1,respectively.The contents of four residual volatile organic solvents in three batches of samples were consistented with the specification requirements.Conclusion:This method is accurate,sensitive,reliable and suitable to analyze the tested solvents.
出处 《中国新药杂志》 CAS CSCD 北大核心 2004年第S1期1359-1361,共3页 Chinese Journal of New Drugs
关键词 阿德福韦酯 气相色谱法 乙腈 二氯甲烷 异丙醚 甲苯 adefovir dipivoxil Head space-gas chromatography acetonitrile dichloromethane iso-prop ether toluene
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