高效离子交换色谱-电化学检测法测定米卡芬净原料中盐酸羟胺  

Determination of Hydroxylamine Hydrochloride in Micafungin by High Performance Ion Exchange Chromatography with Electrochemical Detection

作　　者：高燕霞 徐艳梅 闫凯 韩彬 高凡钦 Gao Yanxia;Xu Yanmei;Yan Kai;Han Bin;Gao Fanqin(Hebei Institute for Drug Control,Shijiazhuang 050011,China;Thermo Scientific Technology(China)Co.Ltd.)

机构地区：[1]河北省药品医疗器械检验研究院,石家庄050011 [2]赛默飞世尔科技(中国)有限公司

出　　处：《中国药师》2021年第4期734-737,共4页China Pharmacist

摘　　要：目的:建立高效阳离子色谱-电化学法测定米卡芬净原料中残留的盐酸羟胺的方法。方法:以IonPac CS16(250 mm×5 mm)色谱柱进行分离,采用100 mmol·L-1甲磺酸溶液为淋洗液梯度洗脱,流速为1.0 ml·ml-1;柱后中和试剂为500 mmol·L-1氢氧化钠溶液,流速为0.3 ml·min-1。采用电化学检测器进行检测,电极材料为金电极,参比电极为pH-Ag/AgCl复合电极,电位波形为氨基酸六电位,柱温30℃,进样体积25μl。结果:羟胺与供试品主峰的分离度良好,羟胺在0.004 2~4.2μg·ml-1范围内线性关系良好(r=1.000 0),检出限(LOD)为0.06 ng。结论:该方法操作简单、专属性强、灵敏度高、重复性好,可用于米卡芬净中痕量羟胺残留的检测。Objective: To establish a method of high performance ion exchange chromatography with electrochemical detection for determining residual hydroxylamine hydrochloride in micafungin. Methods: The sample was separated on an analytical column Ion Pac CS16(250 mm×5 mm),and then analyzed by an external standard method. Gradient elution was performed using 100 mmol·L-1 mesylate solution,and the flow rate was 1.0 ml · ml-1. The post-column neutralization reagent was 500 mmol ·L-1 sodium hydroxide solution at a flow rate of 0.3 ml ·min-1. The electrode was made of gold,the reference electrode was ph-AG/Ag Cl composite electrode,the potential waveform was six potential of amino acid,the column temperature was 30℃,and the volume of injection was 25 μl.Results: The results showed that within the concentration range of 0.004 2-4.2 μg·ml-1,the calibration curves were linear with the correlation coefficient of 1.000 0. The detection limit was 0.06 ng for hydroxylamine hydrochloride. Conclusion: The method is simple,effective,sensitive and selective,and suitable for the determination of hydroxylamine hydrochloride in micafungin.

关 键 词：离子色谱 安培检测器 米卡芬净 盐酸羟胺 

分 类 号：R927.1[医药卫生—药学]