摘要
建立了液相色谱-串联质谱法测定焙烤食品中8种防腐剂含量的方法。样品经正己烷去除油脂,并去掉有机层,用蛋白沉淀剂和无水乙醇混合溶液进行提取,离心并定容。取样液经HLB固相萃取柱净化,氮吹浓缩后用甲醇水溶液溶解,以乙腈和5 mmol/L乙酸铵溶液为流动相,采用液相色谱质谱仪检测。苯甲酸、山梨酸、脱氢乙酸、纳他霉素、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯8种防腐剂在0.01~50 mg/kg范围内线性良好,相关系数在0.99867~0.99984之间,检出限为0.01~0.10 mg/kg,定量限为0.04~0.40 mg/kg,样品加标回收率为82.5%~110.5%,相对标准偏差为4.7%~9.6%。建立的方法可同时测定8种目标物,方法准确度高,稳定性可靠,适用于焙烤食品中多种防腐剂的高通量检测。
This study analyzed eight preservatives in baked foods using liquid chromatography-tandem mass spectrometry(LC-MS/MS).The procedure was as follows:the grease and organic layers were removed using hexane then followed by sample extraction,centrifugation,and resolution using the mixture of protein precipitant and absolute ethanol.The sample solution was further purified using HLB solid phase extraction column and a high concentration of nitrogen was blown over the sample.Moreover,the residue was dissolved in 1 mL of 50% methanol solution and the organic membrane was passed through a 0.22μm filter.Acetonitrile and 5 mmol/L ammonium acetate solution were detected by liquid chromatography mass spectrometer and used as mobile phase.The results showed that eight preservatives including benzoic acid,sorbic acid,dehydroacetic acid,natamycin,methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,propyl p-hydroxybenzoate,and butyl p-hydroxybenzoate showed good linearity in the range of 0.01-50 mg/kg.And the correlation coefficient,limit of detection,limit of quantitation,recovery,and relative standard deviation were 0.99867-0.99984,0.01-0.1 mg/kg,0.04-0.4 mg/kg,82.5%-10.5%,and 4.7%-9.6%,respectively.The LC-MS could test above eight preservatives with good recovery,steady precision,and accurate detection limit.This is suitable for high-throughput detection of multiple kinds of preservatives in food.
作者
李青
蓝梦哲
宋光林
王大霞
上官佳
LI Qing;LAN Mengzhe;SONG Guanglin;WANG Daxia;SHANG Guanjia(GRG Metrology and Test(Hu Nan)Co.,Ltd,Changsha 410013,China;Guangzhou GRG Metrology and Test Co.,Ltd,Guangzhou 510335,China;Guizhou Academy of Testing and Analysis,Guiyang 550002,China;Hunan Testing Institute of Product and Commodity Supervision,Changsha 410007,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2020年第11期283-287,共5页
Food and Fermentation Industries
基金
贵州省科技计划项目(黔科合服企[2019]4001)
贵州省科技计划项目(黔科合支撑[2019]2451号)
广州市科技计划项目(201803020044)。
关键词
液相色谱-串联质谱
固相萃取
焙烤食品
防腐剂
liquid chromatography-tandem mass spectrometry
baked foods
preservatives
solid phase extraction
