超高效液相色谱-高分辨质谱法测定蜂蜜中12种有机磷酸酯类阻燃剂  

Determination of 12 organophosphate esters in honey by ultra-high-performance liquid chromatography-high-resolution mass spectrometry

作　　者：张弛 申慧婧 陈达炜 吴永宁 ZHANG Chi;SHEN Huijing;CHEN Dawei;WU Yongning(School of Food and Health,Beijing Technology and Business University,Beijing 100048,China;China National Center for Food Safety Risk Assessment,Beijing 100021,China)

机构地区：[1]北京工商大学食品与健康学院,北京100048 [2]国家食品安全风险评估中心,北京100021

出　　处：《中国食品卫生杂志》2024年第12期1342-1348,共7页Chinese Journal of Food Hygiene

基　　金：国家重点研发计划(2023YFF1105301)。

摘　　要：目的建立一种超高效液相色谱-高分辨质谱检测蜂蜜中12种有机磷酸酯(OPEs)类阻燃剂的方法。方法采用糖诱导乙腈-水液液萃取体系提取、富集和净化分析目标物,以甲醇-甲酸水进行梯度洗脱,采用HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,高分辨质谱靶向单一离子监测模式结合同位素内标法进行定量。结果在0.2~20μg/L范围内,12种OPEs呈良好线性关系(R2>0.99),方法检出限为0.05~0.3μg/kg,定量限为0.1~0.9μg/kg,3个不同加标水平的回收率为86.2%~119.5%,相对标准偏差为1.24%~8.16%。在16份蜂蜜样品的检测分析中,磷酸三苯酯的检出率达100%,浓度范围为1.7~11.8μg/kg,磷酸三乙酯的检出率为50%,浓度范围为未检出~1.5μg/kg。结论该方法操作便捷,重现性好,灵敏度高,为蜂蜜中OPEs的痕量检测提供了技术支撑。Objective To develop a method for the determination of 12 organophosphate esters(OPEs)fire retardants in honey by ultra-high-performance liquid chromatography-high-resolution mass spectrometry.Methods The samples were enriched,extracted and cleaned-up by a sugar-induced acetonitrile-water liquid-liquid extraction system,eluted with a gradient of methanol-formic acid-water,and then separated on a HSS T3 chromatographic column(2.1 mm×100 mm,1.8μm).The analytes were determined by high-resolution mass spectrometry in the targeted single-ion monitoring mode,with the quantification by isotope internal standard method.Results The linearity of the 12 OPEs,with R²>0.99,was observed from 0.2 to 20μg/L,while the range of the LODs and the LOQs were 0.05-0.3μg/kg and 0.1-0.9μg/kg,respectively.Recoveries of the 12 OPEs at three different spiked levels ranged from 86.2%to 119.5%,with RSDs ranging from 1.24%to 8.16%.Analysis of 16 honey samples revealed 100%detection of TPhP at concentrations ranging from 1.7 to 11.8μg/kg and 50%detection of TEP at levels from LOD to 1.5μg/kg.Conclusion The method is convenient,reproducible,sensitive and suitable for the trace determination of OPEs in honey.

关 键 词：有机磷酸酯类 糖诱导液液萃取 蜂蜜 超高效液相色谱-高分辨质谱法 

分 类 号：R155[医药卫生—营养与食品卫生学]