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投稿时间：2015-09-29
投稿时间：2015-09-29
中文摘要: 改进 3 种 N-亚硝胺（N-亚硝基二乙胺，NDEA；N-亚硝基二甲胺，NDMA；N-亚硝基吡咯烷，NPYR）的测定方法。 以固相微萃取（SPME）为样品萃取方式，配备氮磷检测器的气相色谱仪（GC-NPD）为检测工具，研究 3 种 N-亚硝胺 （NDEA、NDMA、NPYR）的测定方法。以 PDMS/DVB/CAR 为萃取头，萃取温度 50 ℃、搅拌速度 400 r/min、萃取时间 30 min、盐离子浓度 0.20 g/mL 时 NDEA 能得到最大的萃取面积。对 3 种 N-亚硝胺的线性分析得出，NDEA 的测定在 10 ng/mL~100 ng/mL 时线性关系为 0.994；NDMA 在 10 ng/mL~100 ng/mL 时的线性关系为 0.912；NPYR 在 0~10 ng/mL 时 没有表现出明显线性关系。采用 SPME，结合 GC-NPD 测定 N-亚硝胺的方法，对 NDEA 的测定灵敏度最高，RSD 为6.7 %，加标回收率为 89.7 %，最低检出限（LOD）0.67 ng/mL，可以满足肉制品中 NDEA 的定量测定。
Abstract:To improve the test method of N-nitrosamines including NDEA，NDMA and NPYR. The experiment used solid -phase microextraction （SPME） as the extraction method， GC -NPD （gas chromatograph with nitrogen and phosphorus detector） as the detection tool to determine the volatile nitrosamines. Taking PDMS/ DVB/CAR as the extraction， when the extraction temperature was 50 ℃ ， stirring speed was 400 r/min， extraction time was 30 min and the concentration of salt ions was 0.20 g/mL， it could get the largest area of NDEA. We found that when the concentration of NDEA was from 10 ng/mL to 100 ng/mL， it could get the best linear， which reached 0.994. When the concentration of NDMA was from 10 to 100 ng/mL， the linear was better， reached 0.912， and NPYR didn't show clear linear relationship in the concentration range from 0 to 10 ng/mL. To determine the concentration of nitrosamines， solid-phase microextraction with GC-NPD had a good sensitivity of NDEA， RSD was 6.7 %， the recovery rate was 89.7 %， the lowest detection limit （LOD） was 0.67 ng/mL， which meet the quantitative determination of meat and other food products.
keywords: solid -phase microextraction N -nitrosamines extraction conditions linear relationship meat products
文章编号：201603039 中图分类号： 文献标志码：A
基金项目:山西省自然科学基金项目（2013011033-2）；山西农业大学 引进人才博士科研启动基金（2013YJ34）
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