摘要
目的建立了尿样中碘化物的2-丁酮衍生化、气相色谱-三重四极杆质谱联用测定方法。方法尿样通过乙酸锌和亚铁氰化钾沉淀蛋白及杂质,在酸性条件下,重铬酸钾氧化碘离子为碘单质,再采用丁酮衍生化,经环己烷萃取衍生物,萃取液经过DB-5MS毛细管色谱柱分离,在多反应监测模式下,使用三重四级杆质谱仪外标峰面积法定量检测。结果碘化物在20μg/L～500μg/L相关系数为0. 999 5,本方法检出限为1. 0μg/L,方法定量下限为5. 0μg/L,平均加标回收率为95. 3%～98. 0%,相对标准偏差为2. 9%～4. 1%。本方法与国家标准检测方法中的砷铈分光光度法(WS/T 107—2006)比较,差异无统计学意义(P> 0. 05),对标准物质进行了分析,结果令人满意。结论本方法简单、快速、灵敏,可以用于尿样中碘化物的测定。
Objective To develop a method for the determination of iodide in urine by gas chromatography-triple quadrupole mass spectrometry after butanone derivatization.Methods Protein and other impurities were first precipitated with zinc acetate and potassium ferrocyanide and then under acidic condition,iodine ions in sample solution were oxidized into iodine with potassium dichromate.Iodide in sample solution was derived with butanone,and then extracted with cyclohexane,and finally separated with DB-5MS capillary column and detected with triple quadrupole mass spectrometer in the multiple reaction monitoring(MRM)mode.The quantification was based on external standard method.Results The concentration of iodide showed good linear relation within 20μg/L-500μg/L with the correlation coefficient (r)of 0.9995.The detection limit was 1.0μg/L,and the lowest limit of quantification was 5.0μg/L.The average recovery of the method was within 95.3%- 98.0%,with the relative standard derivations (RSD)of 2.9%-4.1%.Compared with As-Ce catalysis spectrophotometry (WS/T 107-2006),the differences were not statistically significant (P>0.05).And the analysis results of standard reference materials were satisfactory.Conclusion The method is simple,rapid and sensitive,which is suitable for the routine analysis of iodide in urine samples.
作者
代澎
张欣
王璟
刘国杰
DAI Peng;ZHANG Xin;WANG Jing;LIU Guo -jie(Shenyang Center for Disease Control and Prevention,Shenyang,Liaoning 110031,China)
出处
《中国卫生检验杂志》
CAS
2019年第2期163-165,共3页
Chinese Journal of Health Laboratory Technology
关键词
碘化物
尿样
衍生化
气相色谱-三重四极杆质谱法
Iodide
Urine
Derivatization
Gas chromatography -triple quadrupole mass spectrometry
作者简介
代澎(1978-),男,硕士,副主任技师,主要从事理化检验方面的研究。
