SPME-GC-NPD法测定肉制品中挥发性N-亚硝胺  

Determination of Volatile N-Nitrosamines by SPME-GC-NPD in Meat Products

作　　者：杨华[1] 方长发[1] 张甜[1] 马俪珍[2] 

机构地区：[1]山西农业大学食品科学与工程学院,山西太谷030801 [2]天津农学院食品科学与工程学院,天津300384

出　　处：《食品研究与开发》2016年第3期150-155,共6页Food Research and Development

基　　金：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)

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/m L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/m L^100 ng/m L时线性关系为0.994;NDMA在10 ng/m L^100 ng/m L时的线性关系为0.912;NPYR在0~10 ng/m L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/m L,可以满足肉制品中NDEA的定量测定。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/m L, it could get the largest area of NDEA. We found that when the concentration of NDEA was from 10 ng/m L to 100 ng/m L, it could get the best linear, which reached 0.994. When the concentration of NDMA was from 10 to 100 ng/m L, the linear was better, reached 0.912, and NPYR didn＇t show clear linear relationship in the concentration range from 0 to10 ng/m L. 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） was0.67 ng/m L, which meet the quantitative determination of meat and other food products.

关 键 词：SPME N-亚硝胺 萃取条件 线性关系 肉制品 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657[轻工技术与工程—食品科学与工程]