【摘要】 利用微波消解-电感耦合等离子体串联质谱（ICP-MS/MS）技术,建立了一种快速测定蜂蜜中微量Se的方法。在MS/MS模式下设置Q1为（m/z）78、80、82,使用O2作为池气体,设定流速为0.40mL/min,Se⁺与O₂反应后生成SeO+,再将Q2分别设置为（m/z）94、96、98,然后进行测定。研究表明:Q1=78/Q2=94的质量对在0.041⁵μg/L范围内线性关系良好（R=0.9999）,检出限为0.013μg/L,样品加标回收率为89.3%¹06.7%,相对标准偏差（RSD）为1.1%³.6%。另外,比较MS/MS模式和MS模式（Q1作为离子导杆）下消除Ca、K元素产生的多原子离子干扰的差异性以及对Se含量测定的影响。与ICP-MS相比,ICP-MS/MS下采用两级质谱进行质量筛选,并结合O2反应,通过质量转移法能获得良好的灵敏度、更低的检测限、更低的背景等效浓度（BEC）和更准确的检测结果,为类似物质的分析提供了参考。更多还原

【Abstract】 A rapid method for the determination of trace selenium（Se）in honey was established by microwave digestion-inductively coupled plasma tandem mass spectrometry（ICP-MS/MS）.Oxygen was selected as the cell gas in MS/MS mode,and the flow rate was set at 0.40 mL/min.Q1 of three main kinds of Se isotopes was set to（m/z）78,80 and 82,respectively.When Se reacted with O₂ to form SeO⁺,Q2 was set to（m/z）94,96 and 98,respectively.The results showed that analytical calibration curves ranging from 0.041μg/L to 5μg/L for selecting the set of mass pairs of Q1=78/Q2=94 was obtained with good linear correlation coefficient（0.9999）in MS/MS mode.The limits of detection（LOD）was 0.013μg/L.The recoveries for Se at two spiked levels were89.3%-106.7% with relative standard deviations ranging from 1.1% to 3.6%.Furthermore,when the operation condition of MS mode（Q1 as an ion guide rod）was set on ICP-MS/MS mode,the influence on Se content and the difference of eliminating polyatomic interference from Ca and K elements in honey were compared between the two modes.Compared with ICP-MS,the proposed O2 mass shift method of ICP-MS/MS can obtain good sensitivity,lower detection limit,lower background equivalent concentration（BEC）and more accurate result.更多还原