摘要
基于乳化/破乳法,本研究建立了一种气相色谱-串联质谱法定量检测牛奶中12种亚硝胺化合物含量的方法。对滤膜种类、提取剂种类以及提取次数等前处理条件的优化结果如下:滤膜种类为尼龙,提取剂为乙腈,提取次数为2次。样品经乙腈提取,蛋白沉淀,乳化/破乳法除脂后,采用HP-INNOWAX色谱柱分离,采用多反应离子监测(MRM)模式,内标法定量测定亚硝胺含量。结果表明,N-亚硝基吡咯烷(NPYR)的线性范围为2~100 ng/mL,其余亚硝胺化合物在1~100 ng/mL的浓度范围内呈现良好的线性关系,决定系数均大于0.995。在高、中、低3个水平加标试验中,回收率在90.90%~114.30%之间,日内精密度在1.76%~7.62%之间,日间精密度在2.75%~7.71%之间。NPYR的定量限为4μg/kg,其余化合物的定量限均为2μg/kg。方法的精密度与准确度良好,可满足牛奶中12种亚硝胺的准确定量需求。实际样品检测结果显示,6组牛奶样品中均检出了N-亚硝基二苯基胺(NDPhA),含量在4.29~6.67μg/kg之间。
Based on the emulsification/demulsification method,a gas chromatography tandem mass spectrometry method was established for the quantitative determination of 12 nitrosamines in milk.The optimization results of pretreatment conditions such as the type of filter membrane,the type of extractant and the number of extractions were as follows:The type of filter membrane was nylon,the extractant was acetonitrile,and the number of extractions was two times.After acetonitrile extraction,deproteinizing,and degreased by emulsification/demulsification,the samples were separated on the HP-INNOWAX chromatographic column.The content of nitrosamines was quantitatively determined by the internal standard method,using multi-reactive ion monitoring(MRM)mode.The results showed that the linear range of Nnitrosopyrrolidine(NPYR)was 2~100 ng/mL,and the linear range of the other nitrosamines was 1~100 ng/mL.All nitrosamines had good determination coefficient which was greater than 0.995.During the high,medium and low-level fortification experiments,the recovery rate ranged from 90.90%to 114.30%,the intra-day precision ranged from 1.76%to 7.62%,and the inter-day precision ranged from 2.75%to 7.71%.The limit of quantitation(LOQ)of N-nitrosopyrrolidine(NPYR)was 4μg/kg,and the LOQ of other compounds was 2μg/kg.The method was precise and accurate,that met the demand of accurately testing 12 nitrosamines in milk.The test results of the actual samples indicated that N-nitrosodiphenylamine(NDPhA)was detected in six milk samples,and the content ranged from 4.29 to 6.67μg/kg.
作者
童文烽
李劲松
徐巧
李剑
TONG Wenfeng;LI Jinsong;XU Qiao;LI Jian(Hangzhou Puyu Technology Development Co.,Ltd.,Hangzhou 311305,China)
出处
《食品工业科技》
CAS
北大核心
2023年第23期280-286,共7页
Science and Technology of Food Industry
关键词
乳化/破乳法
气相色谱-串联质谱法
牛奶
亚硝胺
方法学
emulsification/demulsification method
gas chromatography tandem mass spectrometry
milk
nitrosamines
methodology