摘要
利用欧盟EN12868方法对市售乳胶气球中的8种挥发性亚硝胺及其前体物的模拟迁移量进行了检测，包括N-亚硝基二甲胺（NDMA），N-亚硝基二乙胺（NDEA），N-亚硝基二丙胺（NDPA），N-亚硝基异丙胺（NDiPA），N-亚硝基二丁胺（NDBA），N-亚硝基哌啶（NPIP），N-亚硝基吡咯烷（NPYR），N-亚硝基吗啉（NMOR）。其中NDMA，NDEA和NDBA3种亚硝胺及其前体物被检出，且均超标。建立了顶空-固相微萃取-气相色谱-质谱法（HS—SPME—GC．MS）快速测定乳胶气球中亚硝胺模拟迁移量的分析方法。样品置于人工唾液40℃浸提1h来模拟气球的使用情况，考察了不同的萃取条件对分离检测的影响，综合评价了4种检测系统的性能。8种亚硝胺的方法检出限为0．26～5．38μg／kg。利用所建方法检测9种市售乳胶气球中亚硝胺的模拟迁移总量为31．37～337．72μg／kg。
Firstly, the migration levels of eight volatile nitrosamines including N-nitrosodimethylamine （ND- MA）, N-nitrosodiethylamine （ NDEA）, N-nitrosodibutylamine （ NDBA）, N-nitrodipropylamine （ NDPA）, N-ni- trosopiperdine （ NPIP）, N-nitropyrrobidine （ NPYR）, N-nitrosomorpholine （ NMOR）, N-nitrodiisopropylamine （NDiPA）, and N-nitrosatable substances in latex balloons from the local market were detected by EN12868 standard method. NDMA, NDEA and NDBA were found and showed high contents. Secondly, a rapid method for the determination of simulant migration of eight nitrosamines was developed using the headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry （HS-SPME-GC-MS）, after the latex balloon samples were treated with artificial saliva at 40℃ for 1 h to simulate the usage of latex balloons by children. Theextraction conditions of solid-phase microextraction including the extraction temperature and the extraction time were optimized, respectively. Four detection systems including gas chromatography - thermal energy analyzer （GC-TEA） with DB-FFAP column, gas chromatography - nitrogen chemiluminescence detector （GC-NCD） with DB-FFAP column, and GC-MS with Rtx-1701 column and DB -5MS column were evaluated. The obtained optimal detection conditions of eight nitrosamines were HS-SPME at 60 ℃ for 60 min assisted with magnetic stir- ring followed by GC-MS with Rtx-1701 column. The detection limits of the method （0. 26 -5.38 μg/kg） and good recoveries of eight volatile nitrosamines were obtained. The developed methods are rapid and simple, with adequate sensitivity and without organic solvent. The method was successfully used to analyze simulant migration of volatile nitrosamines from 9 latex balloons, which the total migration value of them were in the range of 31.37 ~ 337.72 μg/kg.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第1期6-11,共6页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金项目(31301465)
北京市优秀人才培养资助项目(2012D005003000001)
北京工商大学青年教师启动基金项目(QNJJ2012_31)资助
关键词
亚硝胺
迁移
气球
EN12868
固相微萃取
气相色谱-质谱联用
Nitrosamines
Migration
Balloon
EN12868
Solid-phase microextracfion
Gas chromatography- tandem mass spectrometry
作者简介
E-mail：fengdi061S@126．com.
