摘要
本研究建立了高效液相色谱-串联质谱快速测定水产品中水杨酸的分析方法。样品直接采用1%甲酸-乙腈溶液提取,乙腈饱和正己烷除油净化,提取液过膜后采用C18(1.7μm,2.1mm×50mm i.d)色谱柱进行分离,以乙腈-0.10%甲酸水溶液为流动相进行梯度洗脱,电喷雾电离,负离子多反应监测模式检测,外标法定量。结果表明:在所建立的方法条件下,水杨酸在0.5～50ng/mL范围内线性关系良好,相关系数为0.999;检出限为2.5μg/kg;不同水产品(黄鳝、财鱼、草鱼和龙虾)在高、中、低3个添加水平下的平均加标回收率在69.10%～97.30%之间,相对标准偏差在2.30%～13.40%之间(n=6)。本方法简便快速、灵敏度高,在日常检测方面存在一定的优势。采用所建立的方法对实际水产样品中的水杨酸残留进行检测,并对残留来源进行溯源分析,可为食品安全风险性评价提供参考依据。
In this study,a rapid method was developed for determination of salicylic acid in aquatic products by high performance liquid chromatography-tandem mass spectrometry.Samples were directly extracted with 1%formic acid acetonitrile and purified with acetonitrile saturated N-hexane,then separated on a C18(1.7μm,2.1 mm×50 mm i.d)column and eluted with the mobile phase of acetonitrile-0.10%formic acid aqueous solution,and analyzed by mass spectrometry in negative ion multiple reaction monitoring mode and using external standards.The results showed that good linearity was obtained in the range of 0.5~50 ng/mL for salicylic acid under the established method,and the correlation coefficients was 0.999.The limits of detection(LOD)was 2.5μg/kg.The average recoveries of the method was ranged from 69.10%to 97.20%with relative standard deviations ranged from 2.30%to 13.40%in aquatic products(Monopterus albus,Snakehead,grass carp and lobster)at three spiked levels(n=6).This proposed method was advantageous in routine detection of salicylic acid residues in aquatic products for its simplicity and high sensibility.The established method was used to detect salicylic acid residues in real aquatic products,and trace the source analysis of the residues,which can provide a useful guideline for risk assessment of the food safety.
作者
朱晓玲
刘杰
吴婉琴
黄茜
张莉
王会霞
江丰
余婷婷
曹琦
韩智
ZHU Xiao-ling;LIU Jie;WU Wan-qin;HUANG Qian;ZHANG Li;WANG Hui-xia;JIANG Feng;YU Ting-ting;CAO Qi;HAN Zhi(Hubei Provincial Institute for Food Supervision and Test,Hubei Provincial Engineering and Technology Research Centerfor Food Quality and Safety Test,Wuhan 430070,China)
出处
《现代食品科技》
EI
CAS
北大核心
2019年第3期218-224,79,共8页
Modern Food Science and Technology
基金
湖北省自然科学基金项目(2018CFB339)
湖北省食品药品监管系统调研课题(鄂食药监办文[2017]11号)
关键词
高效液相色谱-串联质谱
水产品
水杨酸
来源分析
high performance liquid chromatography-tandem mass spectrometry
aquatic products
salicylic acid
source analysis
