摘要
基于重氮化偶合反应,建立了一种可定量分析氨溴特罗口服溶液中微量成分盐酸克仑特罗含量的方法。采用十八烷基硅烷键合硅胶为固定相,以14%冰乙酸溶液(A)-甲醇(B)为流动相进行梯度洗脱,流速为1.0 mL·min^(-1),柱温为30℃,进样量为100μL,进样器温度为4℃,检测波长为450 nm。经方法学验证,盐酸克仑特罗在0.22~0.59μg·mL^(-1)范围内线性关系良好(相关系数>0.999),加标样品回收率在98.50%~102.06%之间(相对标准偏差<1%,n=9),专属性、回收率、精密度及耐用性均可满足要求,并对各批次样品进行检测,其结果均在95%~105%范围内。本方法具有专属性强、准确度高、耐用性好的优势,适用于微量组分盐酸克仑特罗的含量测定,同时为其质量标准制定及后续研究提供技术支持。
Based on the diazotization coupling reaction,a method for the quantitative analysis of the trace component clenbuterol hydrochloride in ambroxol hydrochloride and clenbuterol hydrochloride oral solution has been established.Using octadecylsilyl-bonded silica gel as the stationary phase,gradient elution was performed with a mobile phase composed of 14%acetic acid solution(A)and methanol(B)at a flow rate of 1.0 mL·min^(-1).The column temperature was maintained at 30℃,the injection volume was 100μL,the injector temperature was set at 4℃,and the detection wavelength was 450 nm.Methodological validation indicated that clenbuterol hydrochloride exhibited a good linear relationship within the concentration range of 0.22 to 0.59μg·mL^(-1)(r>0.999).The recovery for spiked samples ranged from 98.50%to 102.06%(RSD<1%,n=9).Specificity,recovery,precision,and robustness of the method all met the required criteria.Furthermore,results were consistently within the range of 95%to 105%for analysis of various batches.This method demonstrates strengths in specificity,high accuracy,and robust durability,making it suitable for the determination of trace amounts of clenbuterol hydrochloride.Additionally,it provides a solid support for the establishment of quality standards and further research.
作者
陈玉洁
刘圆圆
王盛源
李先福
王增明
张慧
刘楠
尤志浩
郑爱萍
CHEN Yujie;LIU Yuanyuan;WANG Shengyuan;LI Xianfu;WANG Zengming;ZHANG Hui;LIU Nan;YOU Zhihao;ZHENG Aiping(School of Pharmacy,Hebei University,Baoding 071002;State Key Laboratory of National Security Specially Needed Medicines,Academy of Military Medical Sciences,Beijing 100850)
出处
《分析科学学报》
北大核心
2025年第4期467-472,共6页
Journal of Analytical Science
关键词
盐酸克仑特罗
重氮化偶合反应
高效液相色谱法
氨溴特罗口服溶液
Clenbuterol hydrochloride
Diazonation coupling reaction
High performance liquid chromatography
Ambroxol hydrochloride and clenbuterol hydrochloride oral solution
