微波消解/ICP-OES法对注射用氟氯西林钠中18种元素杂质的测定

Determination of Eighteen Elemental Impurities in Flucloxacillin Sodium for Injection through ICP-OES with Microwave Digestion

采用了微波消解/电感耦合等离子体发射光谱法(ICP-OES),建立了注射用氟氯西林钠中18种元素杂质的分析方法.在氟氯西林钠样品中加入浓硝酸后进行微波消解,再通过ICP-OES分析.采用垂直观测模式有效减少了易电离元素电离效应的干扰.该方法的线性良好,线性相关系数大于0.998,检出限为0.000 1~0.032 1 mg/L,重复性和精密度的相对标准偏差均小于10%,加标回收率在82.9%-105.7%.采用该方法对3批注射用氟氯西林钠进行检测,样品中元素杂质的含量符合ICH-Q3D与USP通则<232>的规定.该方法的灵敏度和重复性好、准确度高、分析速度快,为注射用氟氯西林钠产品的质量控制提供了技术参考.

The microwave digestion/inductively coupled plasma method(ICP-OES)was used to determine 18 elemental impurities in flucloxacillin sodium for injection.The flucloxacillin sodium sample was digested with microwave after addition of concentrated nitric acid and determined with ICP-OES.The vertical observation mode was used to effectively reduce the interference of ionization effects for the easily ionized elements.The linear relationship of the proposed method was good and the coefficients were over 0.998.The limits of detection ranged from 0.0001 to 0.0321 mg/L.The relative standard deviations of repeatability and precision were less than 10%.The recoveries were in the range from 82.9%to 105.7%.Three batches of flucloxacillin sodium for injection were examined,and the contents of these elemental impurities in these samples met the requirements in ICH-Q3D and USP General Principle<232>.This proposed method showed good sensitivity and precision,high accuracy and fast analysis speed,and would serve as a reliable method for quality control of flucloxacillin sodium for injection.