离子色谱法测定化学对照品中盐酸盐的含量  

Determination of hydrochloride salt content in the chemical reference standards by ion chromatography

作　　者：张才煜[1] 张晓栋 宁保明[1] 吴建敏[1] 何兰[1] ZHANG Cai-yu;ZHANG Xiao-dong;NING Bao-ming;WU Jlan-min;HE Lan(National Institutes for Food and Drug Control, Beijing 102269, China;Changzhou Institute for Drug Control, Changzhou 213002, China)

机构地区：[1]中国食品药品检定研究院,北京102269 [2]常州市食品药品监督检验中心,常州213002

出　　处：《药物分析杂志》2018年第6期1005-1008,共4页Chinese Journal of Pharmaceutical Analysis

基　　金："重大新药创制"科技重大专项(2015ZX09303001)

摘　　要：目的:建立离子色谱-抑制电导检测法测定化学对照品中盐酸盐的含量。方法:以维生素BT、盐酸克仑特罗,盐酸胺碘酮杂质Ⅰ等化学对照品为例,采用DIONEX Ion Pac AS18(250 mm×4 mm)阴离子交换色谱柱,以22 mmol·L^(-1)氢氧化钾溶液为淋洗液等度洗脱,抑制电导检测器检测,测定上述含盐酸盐对照品原料中氯离子的含量,同时本文对化学对照品标定中成盐情况对赋值的影响进行了深入的探讨。结果:该方法在0.002~0.04 mg·mL^(-1)浓度范围内线性关系良好(r=0.999 9),盐酸克仑特罗在3个水平的加样回收率分别为100.5%、99.6%与100.8%,回收率良好。维生素BT(批号100393-201402)、盐酸克仑特罗(批号100072-A)、盐酸克仑特罗USP对照品(批号F01214)、盐酸胺碘酮杂质Ⅰ(批号101399-201601)原料中氯离子中氯离子含量分别为17.54%、11.03%、10.86%、20.33%,与理论值基本一致。而盐酸克仑特罗(批号100072-B)含量为9.09%,与理论值不一致,成盐不完全。结论:本文建立的离子色谱法准确、灵敏,可用于化学对照品中盐酸盐的成盐比例与含量的测定。Objective：To establish an ion chromatography method with suppressed conductivity detection for the hydrochloride salt determination in the chemical reference standards.Methods：The hydrochloride salt content of vitamin BT,clenbuterol hydrochloride and amiodarone hydrochloride impurity Ⅰ was determined.The Cl-was determined by using a DIONEXIon Pac AS18（250 mm×4 mm）anion exchange column with the elution of 22 mmol·L^-1 potassium hydroxide solution at an isocratic elution program.and the influence of the salt content on the chemical reference standards value is also discussed.Results：A good linear relationship was observed in the concentration range of 0.002-0.04 mg·mL^-1（r=0.999 9）,the average recoveries of clenbuterol hydrochloride were100.5%,99.6% and 100.8% at three spiked levels.The contents of hydrochloride in vitamin BT（lot NO.100393-201402）,clenbuterol hydrochloride（lot NO.100072-A）,clenbuterol hydrochloride RS（USP F01214）,amiodarone hydrochloride impurity Ⅰ and in clenbuterol hydrochloride were 17.54%,11.03%,10.86%,20.33%,and 9.09%,respectively.Conclusion：The method is accurate,sensitive,simple,which provides a reliable analytical method for the control of hydrochloride salt content in the chemical reference standards.

关 键 词：离子色谱法 化学对照品 盐酸盐 盐酸克仑特罗 盐酸胺碘酮杂质Ⅰ 维生素BT 

分 类 号：R917[医药卫生—药物分析学]