摘要
建立了一种离子色谱法测定齐多夫定原料药中的痕量叠氮根离子。采用Dionex Ion Pac AS11-HC阴离子分析柱(250×4 mm);以10 mmol/L KOH淋洗液进行等度洗脱;流速为1.0 m L/min;柱温为30℃;进样体积为25μl。该方法条件下,叠氮根与溶液中共存的阴离子能够实现良好分离。叠氮根在0.007~0.135μg/m L范围内呈现良好的线性关系(r=0.9996),加样回收率在97.2%~102.5%之间,检测限为0.002μg/m L。建立的方法简便、灵敏、准确、专属性强、耐用性好,适用于齐多夫定原料药中痕量叠氮根的检测,同时为齐多夫定合成反应中的叠氮工艺优化提供科学依据。
An ion chromatography（IC） method was established for the determination of azide in zidovudine. A Dionex Ion Pac AS11-HC column（250 × 4 mm） was used,with the mobile phase of10 mmol/L KOH eluent generator solution in an isocratic elution. The flow rate was 1. 0 m L/min,the column temperature was 30℃ and the injection was 25 μl. The results showed that all anions can be separate successfully from azide. The calibration curve was in good linearity for azide ranged from0. 007 μg/m L to 0. 135 μg/m L（r = 0. 9996）. The recovery rate was from 97. 2% to 102. 5%,the detection limit was 0. 002 μg/m L. The method is simple,accurate,sensitive with a good specialization and durability which can be used for the determination of azide in zidovudine and also provide scientific data for azide＇s optimization in synthesis of zidovudine.
作者
陆静
李悦
李春刚
LU Jing;LI Yue;LI Chun-gang(Institute of Pharmaceutical Industy,China 201203;Shanghai Shyndec Pharmaceutical Instrumental Analysis ＆ Research Center,Shanghai State Institute of Pharmaceutical Industry,Shanghai（Haimen）Co.,Ltd.,Haimen 226133)
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第8期964-967,共4页
Chinese Journal of Analysis Laboratory
