离子色谱法检测甲氧胺盐酸盐合成过程中的两种二磺酸盐  

Determination of Two Disulfonates in the Synthesis Process of Pharmaceutical Intermediates with Ion Chromatography

作　　者：于忠飞 丛静 赵春华 盖学武 

机构地区：[1]威海市高新区产品质量监督检验所,山东威海264209 [2]诺安检测服务(青岛)有限公司,山东青岛260012 [3]安徽皖仪科技股份有限公司,安徽合肥230088

出　　处：《中国仪器仪表》2013年第12期66-68,共3页China Instrumentation

摘　　要：建立测定羟胺二磺酸盐和甲氧胺二磺酸盐的离子色谱法,并将该方法用于甲氧胺盐酸盐的质量控制。使用抑制型电导检测离子色谱,通过考察不同浓度的Na2CO3和NaHCO3流动相体系对分离效果的影响,选择最适宜的流动相为3.0mmol/L Na2CO3+3.8 mmol/L NaHCO3。两种二磺酸盐的检测线分别为0.15和0.20mg、kg,加标回收率分别为97.8%和98.7%;方法重现性较好,RSD(n=5)低于3%,所建方法适用于甲氧胺盐酸盐的磺酸盐质量控制。A new ion exchange chromatography method of determination of hydroxylamine disulfonate and methoxamine disulfonate is established with suppressed conductivity detector and Na2CO3/NaHCO3 as elution. And the method is used for quality control of pharmaceutical intermediates. By examining the different concentrations of Na2CO3 and NaHCO3 mobile phase on the separation effect, 3.0 mmol/L Na2CO3＋3.8mmol/L NaHCO3 was chosen as the most suitable mobile phase. The recoveries of two disulfonates were 97.8% and 98.7% respectively; Good method reproducibility is obtained, and RSD （n = 5） is less than 3%.

关 键 词：离子色谱 甲氧胺盐酸盐 羟胺二磺酸盐 甲氧胺二磺酸盐 

分 类 号：TQ423[化学工程]