摘要
目的建立QuEChERS净化技术结合超高效液相色谱-串联质谱法同时测定主要肉类与谷物类食品中8种有机磷酸酯类阻燃剂的分析方法。方法采用Agilent EC-C18(3 mm×150 mm,2.7μm)色谱柱,流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速为0.4 mL/min,电喷雾离子源正离子(positive electrospray ionization,ESI+)模式,多反应监测(multiple reaction monitoring,MRM)模式检测。结果8种有机磷酸脂类阻燃剂分离良好,在1.0~50.0 ng/mL范围内具有良好线性关系,相关系数均大于0.99;检出限均为1.0μg/kg;定量限均为2.0μg/kg;方法回收率为70.0%~119.6%,相对标准偏差为0.2%~12.7%。结论本研究建立的方法前处理简单、快速、萃取效率高,并成功应用于食品(谷物、畜肉)中有机磷酸脂类阻燃剂的分析检测。
Objective To establish an analytical method for the simultaneous determination of 8 kinds of organophosphate ester flame retardants of major meat and cereal food products by QuEChERS purification technology coupled with ultra performance liquid chromatography-tandem mass spectrometry.Methods Separation was achieved on a Agilent EC-C18 column(3 mm×150 mm,2.7μm)with a mobile phase consisting of 0.1%formic acid aqueous solution and acetonitrile under gradient elution at a flow rate of 0.4 mL/min.Detection was performed in positive electrospray ionization(ESI+)mode with multiple reaction monitoring(MRM).Results The 8 kinds of organophosphate ester flame retardants exhibited good separation and showed excellent linearity in the range of 1.0–50.0 ng/mL,with correlation coefficients all greater than 0.99.The limits of detection and limits of quantitation were 1.0μg/kg and 2.0μg/kg,respectively.The recoveries of this method were 70.0%–119.6%,and the relative standard deviations were 0.2%–12.7%.Conclusion The established method is simple,rapid and highly efficient in extraction,and has been successfully applied to the analysis of organophosphate ester flame retardants in food samples(including cereals and meat products).
作者
侯俐南
陈静
吕沈亮
韩宇
童仁平
陈燕
HOU Li-Nan;CHEN Jing;LV Shen-Liang;HAN Yu;TONG Ren-Ping;CHEN Yan(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)
出处
《食品安全质量检测学报》
2025年第16期75-85,共11页
Journal of Food Safety and Quality
