摘要
分别考察了萃取溶剂的选择,吸附剂C18和PSA用量。将样品剪成约1cm×1cm左右的碎片并冷冻粉碎,过18目分样筛。样品用10mL二氯甲烷,在30℃条件下超声30min,萃取液经100mg吸附剂C18和100mg PSA净化,离心。上清液用毛细管色谱柱DB-WAX(30m×0.32mm×0.50μm)分离,采用GC/MS选择离子检测,外标法定量。结果表明:N-亚硝基二乙基胺在0.05~4.00mg/L的浓度范围内,线性良好,相关系数(r)为0.9994,方法检出限(LOD)和定量限(LOQ)分别为0.5mg/kg和1.0mg/kg;加标平均回收率在90.2%~98.6%之间,相对标准偏差RSD在2.3%~6.8%之间。该方法样品前处理简单,分析速度快。
The selection of extraction solvents,the amount of adsorbent C18 and PSA were examined,respectively.The sample was cut into approximately 1cm×1cm fragments,frozen and crushed,and passed through an 18 mesh sample sieve.The sample was treated with 10mL of dichloromethane and ultrasound at 30°C for 30minutes.The extract was purified with 100mg of adsorbent C18 and 100mg of PSA,and centrifuged.The supernatant was separated byDB-WAX(30m×0.32mm×0.50μm)quartz capillary column.The samples were detected by GC-MS and quantified by external standard method.The results showed that N-nitrosodiethylamine showed good linearity in the concentration range of 0.05-4.00mg/L,and the correlation coefficient(r)was 0.9994.The limits of detection(LOD)and the limits of quantitation(LOQ)was 0.5mg/kg and 1.0mg/kg,respectively.The average recovery rate ranged from 90.2%to 98.6%,and the relative standard deviations(n=6)ranged from 2.3%to 6.8%.The sample pretreatment is simple,and the analysis is rapid.
作者
唐诗俊
马俊辉
胡丹
周良春
Tang Shijun;Ma Junhui;Hu Dan;Zhou Liangchun(Chengdu Institute of Product Quality Inspection and Research Co.,Ltd.,Chengdu,Sichuan 610100,China;Sichuan Institute of Product Quality Supervision,inspection and Testing,Chengdu,Sichuan 610100,China;Chengdu Institute of Product Quality Supervision and Inspection,Chengdu,Sichuan 610100,China)
出处
《分析仪器》
CAS
2024年第3期20-24,共5页
Analytical Instrumentation
基金
四川省市场监督管理局科技计划项目《儿童接触用橡胶制品有毒有害关键物质定值研究及标准化应用》,项目编号:SCSJS2022009。
关键词
分散固相萃取
气相色谱-质谱法
N-亚硝基二乙基胺
橡胶
Dispersion solid-phase extraction
Gas chromatography-mass spectrometry
N-nitrosodiethylamine
Rubbe
作者简介
唐诗俊,男,硕士,高级工程师,E‐mail:176138075@qq.com;通讯作者:马俊辉,男,高级工程师,主要研究方向:包装材料检验检测。
