摘要
建立了固相萃取-液相色谱/串联质谱(solid phase extraction-liquid chromatography-tandem mass spectrometry,SPE-LC/MS)同时分析静宁烧鸡中14种杂环胺(heterocyclic amines,HAAs)含量的方法。试验首先优化了14种HAAs的仪器参数,待测样品以乙酸乙酯和NaOH提取,经PRS和C18固相萃取小柱串联净化,V(甲醇)∶V(氨水)=19∶1洗脱,将洗脱液混匀过有机滤膜上机检测。结果表明,14种HAAs在1~500μg/L线性良好,相关系数均不低于0.999,检出限(S/N=3)为0.06~0.17μg/kg,定量限(S/N=10)为0.19~0.58μg/kg。14种HAAs在加标水平为20、50、100μg/L时的回收率分别为85.75%~99.14%、85.95%~101.17%、83.04%~103.78%。结果显示该方法线性范围宽、精密度和准确度较高、分析时间短、净化效果好、可满足肉制品中多种HAAs含量同时检测的要求。
A solid phase extraction-liquid chromatography-tandem mass spectrometry(SPE-LC/MS)method was established to sim-ultaneously analyze the contents of 14 heterocyclic amines(HAAs)in Jingning traditional braised chicken.This study firstly optimized the instrument parameters of 14 HAAs,and the meat samples were extracted with ethyl acetate and NaOH,purified by PRS and C18 cartrid-ges in series,and eluted with methanol-ammonia(19∶1,V/V).The eluate was mixed and tested on an organic filter.The results showed that the 14 HAAs had good linearity in the concentration range of 1-500μg/L,the correlation coefficient was not less than 0.999,the detection limit(S/N=3)was 0.06-0.17μg/kg,the limit of quantification(S/N=10)was 0.19-0.58μg/kg.The recoveries of 14 HAAs at spiked levels of 20,50,and 100μg/L were 85.75%-99.14%,85.95%-101.17%,83.04%-103.78%,respectively.The results showed that the method had a wide linear range,high precision and accuracy,short analysis time,and good purification effect,which could meet the requirements of simultaneous detection of multiple HAAs residues in meat products.
作者
田铸
陈敬敬
张丹
张珍
陈骋
师希雄
TIAN Zhu;CHEN Jingjing;ZHANG Dan;ZHANG Zhen;CHEN Cheng;SHI Xixiong(Food Science and Engineering College,Gansu Agricultural University,Lanzhou 730070,China;Gansu Provincial Key Lab of Aridland Crop Science,Gansu Agricultural University,Lanzhou 730070,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2022年第22期285-291,298,共8页
Food and Fermentation Industries
基金
甘肃省优秀研究生“创新之星”项目(2021CXZX-415)
甘肃传统肉制品绿色制造技术研究及产业化示范(20YF3NA014)。
关键词
烧鸡
杂环胺
固相萃取
液相色谱-质谱联用
肉制品
braised chicken
heterocyclic amine
solid phase extraction
liquid chromatograph mass spectrometer(LC-MS)
meat products
