固相萃取净化—高效液相色谱法测定肉制品中的9种N-亚硝基化合物  

Determination of Nine N-Nitroso Compounds in Meat Products by Solid Phase Extraction Purification and High Performance Liquid Chromatography

作　　者：蔡鲁峰 李娜[1,2] 杜莎 谭雅[1] 李珂[1] 王远亮[1] 

机构地区：[1]湖南农业大学食品科学技术学院,食品科学与生物技术湖南省重点实验室,湖南长沙410128 [2]湖南省商业技师学院烹饪系,湖南株洲412000

出　　处：《食品科学》2016年第12期217-221,共5页Food Science

基　　金：湖南省战略性新兴产业项目(2014GK1034);湖南省自然科学基金项目(11JJ4019);湖南省科技计划项目(2015WK3015);湖南农业产业技术体系加工岗位专家项目;公益性行业(农业)科研专项(201303082)

摘　　要：建立采用固相萃取—高效液相色谱法同时测定肉制品中9种N-亚硝基化合物的方法。以甲醇为提取剂,60℃条件下超声提取,经CNWBOND HC-C（18）固相萃取柱净化后,采用AQ-C（18）色谱柱分析。甲醇和超纯水为流动相实现了待测物的良好分离,紫外检测器检测,结合保留时间和光谱图定性,外标法定量。结果表明：9种N-亚硝基化合物线性关系良好,相关系数均大于0.99;方法定量限（R（SN）=10）为0.047-0.097μg/g;回收率为72.6%-97.6%;相对标准偏差（n=6）为3.1%-7.9%。此方法前处理简单、回收率高、精密度好,适用于肉制品中9种N-亚硝基化合物的同时测定。A solid-phase extraction （SPE）-high performance liquid chromatography （HPLC） method has been developed forsimultaneous determination of 9 N-nitroso compounds （NOCs） in meat products. The analytes were extracted with methanolat 60 ℃ ultrasonically, purified by a CNWBOND HC-C18 SPE column, and analyzed by HPLC on a Phenomenex AQ-C18column （250 mm × 4.6 mm, 5 μm） employing methanol and ultrapure water as the mobile phase in a gradient elution mode.The 9 N-nitroso compounds were qualitatively determined by retention time, and confirmed by ultraviolet spectroscopy.The results indicated that the calibration curves of the target analytes displayed good linearity with correlation coefficients（r） greater than 0.99. The method limits of quantification （MLOQ） for the target analytes ranged from 0.047 to 0.097 μg/g（RSN =10）. The recoveries were in the range between 72.6% and 97.6%, and the precision （relative standard deviation, RSD）ranged from 3.1% to 7.9% （n = 6）.

关 键 词：N-亚硝基化合物 固相萃取 高效液相色谱 肉制品 

分 类 号：TS207.3[轻工技术与工程—食品科学]