高效液相色谱-共振瑞利散射联用检测人体尿液中的法莫替丁与雷尼替丁  

Determination of Famotidine and Ranitidine in Human Urine by High Performance Liquid Chromatography-Resonance Rayleigh Scattering

作　　者：陈方 张钰玉 龙登莹 鲜红 彭敬东[2] CHEN Fang;ZHANG Yu-yu;LONG Deng-ying;XIAN Hong;PENG Jing-dong(School of Chemical and Materials Engineering,Guiyang College,Guiyang 550005,China;School of Chemistry and Chemical Engineering,Southwest University,Chongqing 400715,China)

机构地区：[1]贵阳学院化学与材料工程学院,贵州贵阳550005 [2]西南大学化学化工学院,重庆400715

出　　处：《分析测试学报》2021年第7期1080-1085,共6页Journal of Instrumental Analysis

基　　金：贵阳市科学技术局-贵阳学院科技专项资金(GYU-KYZ(2019~2020)ZZ-01);国家自然科学基金(21277110)。

摘　　要：建立了高效液相色谱(HPLC)与共振瑞利散射(RRS)联用检测人体尿液中法莫替丁(FMTD)和雷尼替丁(RNTD)的方法。柱前分离系统以乙腈与醋酸-醋酸钠缓冲溶液(pH 4.5)为流动相等度洗脱,流速为0.5mL/min,进样量为20μL,柱温为35℃,使用Kinetex 5μm C_(18)液相色谱柱(250 mm×4.60 mm);柱后衍生系统以赤藓红与金属离子Pd(Ⅱ)同时作为探针,探究了柱后衍生的最佳实验条件。结果显示,法莫替丁与雷尼替丁分别在0.024~25μg/mL和0.033~25μg/mL质量浓度范围内线性良好,相关系数(r)分别为0.999 0和0.998 8,检出限(S/N>3)分别为7.3、10.1 ng/mL。采用该方法对已知混合浓度的样品进行测定,加标回收率为97.8%~102%,相对标准偏差(RSD)均不大于5.1%。该方法的可靠性和实用性良好,可用于人体尿液中法莫替丁和雷尼替丁的检测。A high performance liquid chromatography(HPLC)combined with resonance Rayleigh scattering(RRS)was developed for the determination of two H2-receptor blockers,famotidine(FMTD)and ranitidine(RNTD)in human urine.Separation conditions for HPLC were as follows:a volume ratio of 10:90 for acetonitrile and sodium acetic acid(pH 4.5),a flow rate of 0.5 mL/min,a Kinetex5μm C18 column(250 mm×4.60 mm),a sample size of 20μL and a column temperature of 35℃.The optimal experimental conditions were investigated by a new post-column derivation method with metal ion Pd(Ⅱ)and dye erythrin(Ery)as the probes.Results showed that there were good linear relationships for FMTD and RNTD in the ranges of 0.024-25μg/mL and 0.033-25μg/mL,with their correlation coefficients(r)of 0.9990 and 0.9988,respectively.The detection limits(S/N)for FMTD and RNTD were 7.3 ng/mL and 10.1 ng/mL,respectively.This method was used for the determination of a known concentration of mixed samples.The spiked recoveries ranged from 97.8%to 102%,with relative standard deviations no more than 5.1%.Furthermore,the method was successfully applied to detect the content of FMTD in human urine,without any other matrixes in the urine to interfere the RRS signal.Therefore,the method is reliable and practical,and could be used to detect H2-receptor blockers in human urine.

关 键 词：高效液相色谱 共振瑞利散射 H_2受体阻滞剂 法莫替丁 雷尼替丁 尿液 

分 类 号：O657.7[理学—分析化学]