摘要
目的建立一种简单、快速的分散固相萃取-高效液相色谱-串联质谱法测定水果中单乙醇胺(monoethanolamine,MEA)、二乙醇胺(diethanolamine,DEA)和三乙醇胺(triethanolamine,TEA)残留量的分析方法。方法样品均质后以乙醇超声提取,提取液经N-丙基乙二胺(primary secondary amine,PSA)+C_(18)混合分散净化后,采用Accucore polar premium(100 mm×4.6 mm,2.6μm)色谱柱分离,以5 mmol/L甲酸铵-乙腈为流动相梯度洗脱,在电喷雾正离子多反应监测模式下检测,外标法定量。结果单乙醇胺、二乙醇胺和三乙醇胺分别在10.0~1000.0、3.0~1000.0、1.0~1000.0μg/L范围内线性关系良好,相关系数均大于0.996,单乙醇胺、二乙醇胺和三乙醇胺的检出限分别为50.0、15.0和5.0μg/kg,定量限分别为150.0、40.0和15.0μg/kg,3种乙醇胺类化合物在高中低浓度的加标回收率为79.4%~102.1%,重复性精密度为1.4%~9.6%(n=6)。结论该方法具有操作简便、定量准确、灵敏快速的特点,适用于水果中单乙醇胺、二乙醇胺和三乙醇胺的检测确证。
Objective To establish a simple and rapid analytical method for the determination of monoethanolamine(MEA),diethanolamine(DEA)and triethanolamine(TEA)residues in fruits by dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.Methods The samples were homogenized,followed by ultrasonic extraction with ethanol,after the primary secondary amine(PSA)+C_(18) dispersion purification of the extractive solution,the samples were separated using an Accucore polar premium(100 mm×4.6 mm,2.6μm)chromatographic column,and gradient elution was performed using 5 mmol/L ammonium formate-acetonitrile as the mobile phase,and the samples were detected under the electrospray positive ion multiple reaction monitoring mode,and quantified by external standard method.Results The linear relationship of MEA,DEA and TEA were good in the range of 10.0-1000.0,3.0-1000.0 and 1.0-1000.0μg/L respectively,the correlation coefficients were greater than 0.996,the detection limits of MEA,DEA and TEA were 50.0,15.0 and 5.0μg/kg respectively,the quantitation limits were 150.0,40.0 and 15.0μg/kg,respectively.The recoveries of the 3 kinds of ethanolamine compounds at high,medium,and low concentrations were 79.4%-102.1%,and the repeatability precisions were 1.4%-9.6%(n=6).Conclusion This method is simple,accurate,sensitive and rapid,and suitable for the determination and confirmation of MEA,DEA and TEA in fruits.
作者
李秀英
陈伟萍
周朗君
岑建斌
管嘉武
何敏恒
LI Xiu-Ying;CHEN Wei-Ping;ZHOU Lang-Jun;CEN Jian-Bin;GUAN Jia-Wu;HE Min-Heng(Guangzhou Inspection Testing and Certification Group Co.,Ltd.,National Quality Inspection and Testing Center for Processed Foods(Guangdong),Guangzhou 511447,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第1期34-39,共6页
Journal of Food Safety and Quality
基金
广东省市场监督管理局科技计划项目(2020CS03)。
关键词
水果
乙醇胺类
高效液相色谱-串联质谱法
分散固相萃取
fruits
ethanolamines
high performance liquid chromatography-tandem mass spectrometry
dispersive solid-phase extraction
