不锈钢柱管中自制弱阳离子交换整体柱作为固相萃取材料,对尿样中盐酸雷尼替丁进行富集分析。以2.5mmol/LK2HPO4缓冲液作为富集流动相,结合柱切换法实现在线富集药物的同时去除尿液中蛋白等内源性物质。色谱分离条件为:C18反相色谱柱,在流速为1.0mL/min,检测波长为320nm条件下,用CH3OH-2.5mmol/LK2HPO4(2:1,V/V)进行洗脱。实验结果表明,盐酸雷尼替丁在0.05~5.0mg/L浓度范围内线性关系良好(r=0.9994,n=7);绝对回收率在75.0%~85.0%之间;检出限为0.01mg/L;日内、日间精密度(RSD)均小于5.0%,能够满足分析测定要求。本方法避免了繁琐的样品预处理过程,且所制弱离子整体柱可多次重复使用,为生物样品中痕量药物检测提供了一种快速、经济和有效的新方法。
A weak cation exchange monolithic column was prepared in stainless steel column tubule,which was used for analysis and determination of ranitidine hydrochloride as solid phase extraction(SPE) material in urine samples.With the column switch technique,online cleaning up and screening of human urine sample was executed under the condition of 2.5 mmol/L K2HPO4 solutions.Chromatographic operation was performed by reversed-phase HPLC on a C18 column with 1.0 mL/min flow ratio and ultraviolet detection at 320 nm,using an eluting solution consisting of methanol-2.5 mmol/L K2HPO4(2∶1,V/V).Results showed that there was a good linear relationship between the response and the concentration of ranitidine hydrochloride within the range of 0.05-5.0 mg/L(r=0.9994,n=7).The absolutely recovery rate was from 75.0% to 85.0% and the detection limit was 0.01 mg/L.The inter-day RSD and intra-day RSD were less than 5%.This method was suitable for the determination of Ranitidine hydrochloride in human urine,which had avoided tedious pretreatment and provided a fast,economic,repeated and effective method for assaying trace drugs in biologic samples.