柱前衍生-高效液相色谱法测定人尿中硫氰酸盐  

Detecting thiocyanate in human urine by precolumn derivatization-high performance liquid chromatography

作　　者：袁静 阮小林[1] 戎伟丰[1] 胡嘉雯 马安萍 YUAN Jing;RUAN Xiaolin;RONG Weifeng;HU Jiawen(Guangdong Province Hospital for Occupational Disease Prevention and Treatmen;Guangdong Provincial Key Laboratory of Occupational Diseases Prevention and Treatment, Guangzhou, Guangdong 510300, Chin)

机构地区：[1]广东省职业病防治院广东省职业病防治重点实验室,广东广州510300 [2]广东药科大学,510310

出　　处：《中国职业医学》2018年第3期373-376,共4页China Occupational Medicine

基　　金：国家科技支撑计划项目(2014BAI12B01);国家临床重点专科建设项目(2011-09);广东省职业病防治重点实验室(2017B030314152)

摘　　要：目的建立以五氟苄基溴作为柱前衍生试剂,高效液相色谱法测定人尿中硫氰酸盐的方法。方法尿样中硫氰酸盐与五氟苄基溴衍生后,经多孔层120EC-C18色谱柱分离,以乙腈:去离子水(60:40,V/V)为流动相,经高效液相色谱-紫外检测器检测,检测波长为212 nm。结果尿中硫氰酸盐质量浓度为0.05~10.32 mg/L时线性关系良好,线性相关系数为0.999;检出限为6.31μg/L,最低检出浓度为63.10μg/L(以尿样体积0.1 mL计);加标回收率为95.1%~102.9%;批内相对标准偏差(RSD)为0.9%~1.0%,批间RSD为0.9%~2.1%;在4℃样品可保存7 d。结论本法灵敏度高、特异性好、样品前处理简单,可用于职业人群尿中硫氰酸盐的测定。Objective To establish a method for detecting thiocyanate in human urine by high performance liquid chromatography（ HPLC） with 2,3,4,5,6-pentafluorobenzyl bromide as precolumn derivatization reagent.Methods Thiocyanate in human urine was derived with 2,3,4,5,6-pentafluorobenzyl bromide, and separated by poroshell 120EC-C18 column with acetonitrile：deionized water（ 60：40,V/V） as mobile phase.detected by HPLC,Liquid chromatography-UV detector was used for determination.The wavelength was 212.00 nm.Results Good linearity was obtained in the range of 0.05-10.32 mg/L with the correlation coefficient of 0.999.The detection limit was 6.31 μg/L and the minimum detection concentration was 63.10 μg/L（ 0.1 mL urine）.The recovery rate was 95.1%-102.9%.The within-run relative standard deviation（ RSD） and the between-run RSD were 0.9%-1.0% and 0.9%-2.1%,respectively.The urine samples could be stored at 4 ℃ for 7 days.Conclusion This method has high sensitivity,good specificity and sample preparation,which can be used for detecting urine thiocyanate in occupational population.

关 键 词：硫氰酸盐 尿 五氟苄基溴 柱前衍生 高效液相色谱法 

分 类 号：R134.4[医药卫生—劳动卫生]