固相萃取-高效液相色谱法同时测定酱腌菜中N-亚硝基二甲胺(NDMA)和N-亚硝基二乙胺(NDEA)  

Determination of N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) in pickled vegetables by solid-phase extraction and high-performance liquid chromatography

作　　者：张秋菊[1] 崔世勇[1] 曹林波[1] 姜丽华[1] 

机构地区：[1]上海市宝山区疾病预防控制中心,上海201901

出　　处：《中国卫生检验杂志》2010年第11期2687-2689,共3页Chinese Journal of Health Laboratory Technology

基　　金：上海市宝山区科委2008年立项项目(2008-E-31)

摘　　要：目的:建立固相萃取-高效液相色谱法(SPE-HPLC)测定酱腌菜中N-亚硝基二甲胺(NDMA)和N-亚硝基二乙胺(NDEA)的方法。方法:样品经纯水浸取,再经Envi-Carb柱和Lichrolut EN柱净化吸附浓缩后,用甲醇洗脱。以甲醇+水(20+80)为流动相,经Capcell PAK C18色谱柱分离,于228 nm处检测。结果:NDMA和NDEA分别在5 ng/ml～3750 ng/ml和10 ng/ml～5000 ng/ml范围内具有良好的线性,其相关系数均大于0.999,检出限分别为2.5 ng/ml和5.0 ng/ml,实际样品加标回收率分别为92%～98%和91%～101%,相对标准偏差<10%。结论:此法简单、灵敏、准确,可用于同时测定样品中NDMA和NDEA。Objective：A simple and accurate method for determination of N-nitrosodimethylamine（NDMA） and N-nitrosodiethylamine（NDEA） in pickled vegetables by solid-phase extraction and high-performance liquid chromatography（SPE-HPLC） was established.Methods： NDMA and NDEA were lixiviated,cleaned and adsorbed by Envi-Carb column and Lichrolut EN column,then desorbed by methanol.The separation was performed on Capcell PAK C18 column with CH3OH/H2O（20∶80,v/v） as the mobile phase and detected at the wavelength of 228 nm.Results： The linear range was 5 ng/ml～3750 ng/ml and 10 ng/ml～5000 ng/ml for NDMA and NDEA,respectively（r0.999）.The minimum detection limits of NDMA and NDEA were 2.5 ng/ml and 5.0 ng/ml,respectively.The recovery of NDMA and NDEA were 92%～98% and 91%～101%,severally,and the RSD was less than 10%.Conclusion： The proposed method was simple,sensitive and reliable for the determination of NDMA and NDEA.

关 键 词：SPE-HPLC 酱腌菜 N-亚硝基二甲胺 N-亚硝基二乙胺 

分 类 号：O657.72[理学—分析化学]