摘要
本文建立了全自动固相萃取-液相色谱-串联质谱法测定肉类食品中苯乙醇胺A残留量的方法。样品在酶解条件下用乙酸铵缓冲溶液提取,经MCX固相萃取柱全自动固相萃取净化,洗脱液在45℃条件下氮气吹干,加入1.0 mL 0.1%甲酸溶液溶解后上机检测。采用Poroshell 120 EC-C18,100 mm×3.0 mm(i.d.),2.7μm色谱柱分离,在多反应监测模式下进行质谱检测,内标法定量。结果表明,苯乙醇胺A在1.0~100.0μg/L浓度范围内具有良好的线性关系,相关系数r=0.9993,检出限(LOD)为0.2μg/kg,定量限(LOQ)为0.5μg/kg。在不同添加水平下,其平均回收率为90.5%~103.3%,变异系数为2.2%~7.0%。建立的方法能够对样品进行全自动净化,提高了检测效率,适用于肉类食品中苯乙醇胺A残留的检测。
A method for the determination of Phenylethanolamine A residues in meat products by automatic solid phase extraction-liquid chromatography tandem mass spectrometry was established in this paper.The sample was extracted with ammonium acetate buffer solution under enzymolysis condition,and purified by MCX solid phase extraction column in automatic solid phase extraction.The eluent was dried by nitrogen at 45°C,and 1.0 mL 0.1%formic acid solution was added for dissolution and detection.Using Poroshell 120 EC-Cis,100 mm×3.0 mm(i.d),2.7μm chromatographic column separation,the sample was detected in multi reaction monitoring mode of mass spectrometry,and was quantifed by internal standard method.The results indicated that Phenylethanolamine A had a good linear relationship in the concentration range of 1.0-100.0μg/L,with the correlation coefficient of r=0.9993.The detection limit(LOD)was 0.2μg/kg,with the quantification limit(LOQ)0.5μg/kg.At different levels of addition,the average recovery rate were 90.5%-103.3%,and the coeficient of variation were 2.2%-7.0%.The established method can automatically purify the samples,improve the detection efficiency,and is suitable for the detection of Phenylethanolamine A residues in meat products.
作者
倪永付
王勇
高瑞刚
高洁
王鹏
白翔
NI Yong-Fu;WANG Yong;GAO Rui-Gang;GAO Jie;WANG Peng;BAI Xiang(Comprehensive Technical Service Center of Jining Customs,Jining 272000;Qingdao International Travel Healthcare Center(Qingdao Customs Port Outpatient Departments),Qingdao 266001)
出处
《中国口岸科学技术》
2023年第8期54-60,共7页
China Port Science and Technology
关键词
全自动固相萃取
液相色谱-串联质谱
肉类食品
苯乙醇胺A
残留
automated solid phase extraction
liquid chromatography tandem mass spectrometry
meatproducts
Phenylethanolamine A
residues
