尿中N-甲基乙酰胺直接进样-氮磷检测气相色谱分析法  

The Analysis of urinary N-methylacetamide by GC-NPD with a direct injection

作　　者：唐红芳[1] 阮征[1] 刘丹华[1] 王晗[1] 朱海豹[1] 吴昊[1] 钱亚玲[1] 

机构地区：[1]浙江省医学科学院卫生学研究所,杭州310013

出　　处：《中华劳动卫生职业病杂志》2012年第5期386-388,共3页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：卫生部政策法规司卫生标准制订项目（20100308）：浙江省公共卫生检验检测重点学科群项目（XKQ-009-003）;浙江省科技厅项目（2011F10049）

摘　　要：目的建立直接进样-气相色谱法检测尿中N-甲基乙酰胺（NMAC），为研制职业接触二甲基乙酰胺生物限值提供配套检测方法。方法用甲醇稀释经冷冻离心的尿样，分离蛋白沉淀后直接进样，经聚乙二醇毛细管色谱柱程序升温分离，氮磷检测器检测。结果尿中NMAC的线性范围为1．0～250mg／L，相关系数为1．0000；最低检测浓度为0．2mg／L；添加水平为10．58、52．90、211．60mg／L时，NMAC回收率为96．0％-99．4％，平均回收率为97．8％；批内和批间相对标准偏差为1．5％～3．4％。结论本方法简便快速，灵敏准确，适用于DMAC职业暴露人群尿样中NMAC的监测。Objective To establish a method to detect N-methylacetamide （NMAC） concentration in urine of workers occupationally exposed to NMAC with directly injecting the sample into capillary gas chromatography. Methods After frozen urine samples were isolated from precipitation by centrifugation, the aliquot of supernatant was pretreated by protein precipitation with dilution of methanol. The methanol supernatant was separated by Polyethylene Glycol （PEG）capillary columns and detected by nitrogen phosphoraus detector （NPD）. Results Good linearity was obtained in the concentration range of 1.0-250 mg/L. The correlation coefficient was 1.0000. The minimum detection limit of NMAC in urine was 0.2 mg/L. The method recovery rates were 96.0% - 99.4% at three different concentrations. The mean recovery rate was 97.8%. The relative standard deviations （RSD） of intra- and inter-day were between 1.5%-3.4%. Conclusion The method was simple, rapid, selective and sensitive and was applicable to detect the urinary NMAC concentration for monitoring occupational exposure levels.

关 键 词：N-甲基乙酰胺 N N-二甲基乙酰胺 尿 色谱法 气相 

分 类 号：R446.12[医药卫生—诊断学]