研究建立了ICP-MS/MS检测食品中磷、砷和硒含量的检测方法。分析了P、As和Se在检测过程中常见的质谱干扰和电离效率，比较了标准模式（No Gas）、He模式、H2模式、O2模式以及双四极杆等各种检测模式，发现采用O2模式双质谱对P、Se的检测结果最为准确，As采用He模式即可实现精准检测。根据优化后的检测条件，经过Q1时同位素M进入碰撞反应池，与O2反应生成的氧化物MO进入Q2被采集，通过二级质谱质量转移几乎可以彻底消除一切干扰。结果显示，P在2.0~500 μg/L范围内、As和Se在0.5~200 μg/L浓度范围内均具有良好的线性，相关系数均大于0.9995，加标回收显示回收率在94.0~101.5%之间，RSD%不大于2.1%。最终采用该方法对国家标准物质乳粉样品（GBW 10017）、螺旋藻（GBW 10025）进行测定，结果均在标准值范围内。本方法可以满足食品中P、As和Se等元素的精准检测。

A method for the determination of phosphorus, arsenic, and selenium contents in foods by inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS) was established. The common mass spectral interference and ionization efficiency during measurements of phosphorus, arsenic, and selenium were analyzed, and the standard mode (no gas), helium mode, hydrogen mode, oxygen mode, and double quadrupole detection mode were compared. The most accurate results for phosphorus and selenium detection were obtained by using the oxygen mode and dual mass spectrometry, and the helium mode could be used for the accurate detection of arsenic. According to the optimized detection conditions, the isotopes of M entered the collision cell after Q1, and reacted with oxygen to form the oxide MO, which entered into Q2. Mass transfer of the tandem mass spectrum could almost eliminate all interference. The results showed that good linear calibration curves were obtained in the range of 2.0~500 μg/L for phosphorus and 0.5~200 μg/L for arsenic and selenium, and the correlation coefficients were over 0.9995. The recoveries were in the range of 94.0~101.5%, and the relative standard deviations (RSDs%) were not more than 2.1%. Finally, national standard substance milk powder sample (GBW10017) and Spirulina (GBW10025) were analyzed using this method, and the results were all within the standard value range. Therefore, the method can meet the requirements for the accurate detection of phosphorus, arsenic, and selenium in food.

国家质检总局科技计划项目（2015IK255）