肉制品中9种N-亚硝胺测定方法的建立  

Establishment of Methods in Nine Kinds of Volatile N-nitrosamines Determination in Meat Products

作　　者：张建斌 马俪珍 张甜[3] 杨华 Zhang Jianbin;Ma Lizhen;Zhang Tian;Yang Hua(College of Animal Science and Veterinary Medicine,Tianjin Agricultural University,Tianjin 300384;College of Food Science and Bioengineering,Tianjin Agricultural University,Tianjin 300384;College of Food Science and Engineering,Shanxi Agricultural University,Taigu 030801,Shanxi)

机构地区：[1]天津农学院动物科学与动物医学学院,天津300384 [2]天津农学院食品科学与生物工程学院,天津300384 [3]山西农业大学食品科学与工程学院,山西太谷030801

出　　处：《中国食品学报》2020年第5期276-282,共7页Journal of Chinese Institute Of Food Science and Technology

摘　　要：建立超声波提取-固相萃取-气相色谱-氮磷检测(UE-SPE-GC-NPD)和超声波提取-固相萃取-液相色谱-紫外检测(UE-SPE-HPLC-UV)肉制品中9种N-亚硝胺的方法。选取二氯甲烷作为提取试剂,探讨萃取时间、有机溶剂用量和萃取功率对提取效果的影响,比较C18、中性氧化铝和活性炭3种固相萃取柱对超声波提取的目标物的净化作用。结果表明:样品经40 mL二氯甲烷在400 W功率下提取20 min,N-亚硝胺的峰面积达到最大值,即提取效果最好。通过回收率试验选取活性炭固相萃取小柱为样品净化。UE-SPE-GC-NPD的回收率在66.80%~93.89%之间,其精密度在1.39%~3.07%之间。UE-SPE-HPLC-UV的回收率在65.80%~93.20%之间,其精密度均在1.19%~3.42%之间,该方法简便、快速,具有良好的灵敏度、重复性,适用于同时测定肉及肉糜制品中9种N-亚硝胺类化合物的含量。Methods of solid phase extraction and liquid chromatography with ultraviolet detection(SPE-HPLC-UV)for simultaneous determination in meat products of 9 kinds of N-nitrosoamines(NDMA,NMEA,NDEA,NDPA,NDBA,NPIP,NPYR,NMOR and NDpheA)were established.Using dichloromethane as extraction reagent to investigate the effect of extraction consisting of extraction time,solvent amount and extraction power,compared the purification effect of C18,neutral alumina and activated carbon for ultrasonic extraction of sample.The results showed that using 40 mL dichloromethane,400 W,extract 20 min,the peak area of N-nitrosamines reached the maximum.And finally through the recovery experiment selected activated carbon solid-phase extraction as sample purification.The recovery of the method was 86%-99%,and the precision was 1.19%-3.42%,the method is simple and rapid,with good sensitivity,repeatability,and can be applied to simultaneous determination of content in meat products of 9 kinds of N-nitrosamines compounds.

关 键 词：超声波提取 固相萃取 肉制品 N-亚硝胺 萃取条件 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657[轻工技术与工程—食品科学与工程]