尿中二氨基二苯基甲烷的液相色谱-串联质谱测定方法研究  

Determination of methylenedianiline in urine by high performance liquid chromatography-tandemmass spectrometry

作　　者：李添娣 刘奋 潘兴富 陶雪 赵玮 闫慧芳[2] Li Tiandi;Liu Fen;Pan Xintu;Tao Xue;Zhao Wei;Yan Huifang(Shenzhen Prevention and Treatment center for Occupational Diseases, Shenzhen 518001, China)

机构地区：[1]深圳市职业病防治院,518000 [2]中国疾病预防控制中心

出　　处：《中华劳动卫生职业病杂志》2018年第4期308-311,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：深圳市科技计划项目（JCYJ20170307145400143）;深圳市科技计划项目（JCYJ20160429090813380）

摘　　要：目的 建立尿中二苯基甲烷二异氰酸酯（MDI）代谢产物二氨基二苯基甲烷（MDA）的液相色谱-串联质谱测定方法.方法 尿样经硫酸酸化水解,乙腈液液萃取,经Shim-pack XR-ODS色谱柱分离,电喷雾电离质谱检测,外标法定量.结果 MDA在0.05-20.00 μg/L的范围内线性良好,相关系数r为0.999 5,检出限0.02 μg/L,平均回收率为91.0％- 103.4％,相对标准偏差（RSD）在2.7％-7.3％之间.结论 该方法简便、灵敏、准确,可适用于MDI接触人群尿中MDA含量的测定.Objective To develop a method for determination of metabolites of diphenylmethane diisocyanate （MDI） in urine,i.e.methylenedianiline （MDA） by high performance liquid chromatography-tandem mass （LC-MS-MS）.Methods Urine samples were prepared by hydrolyzation with sulfuric acid and extraction by acetonitrile,and then separated on a Shim-pack XR-ODS column,analyzed with high-performance liquid chromatography-tandem mass spectrometry （LC-MS/MS）.The external solvent standard calibration were tested.Results The linearity ranges were 0.05-20.00 μg/L,The related coefficients were 0.999 5.The limit of detection was 0.02 μg/L.The rats of recovery were 91.0%-103.4%.The relative standard deviations were between 2.7%-7.3%.Conclusion The method was sensitive,accurate and suitable for the MDA determination in urine of MDI exposed population.

关 键 词：二氨基二苯基甲烷(MDA) 液相色谱-串联质谱 二苯基甲烷二异氰酸酯(MDI) 尿 

分 类 号：R135[医药卫生—劳动卫生] R446.12[医药卫生—公共卫生与预防医学]