建立了电感耦合等离子体串联质谱(inductively coupled plasma tandem mass spectrometry,ICP-MS/MS)法准确测定水产品中多种痕量重金属元素的分析方法。针对ICP-MS/MS分析中复杂基质所形成的质谱干扰,在MS/MS模式下,向八极杆碰撞反应池(octopole reaction system, ORS)中通入O2为反应气,分析离子Cr+、Ni+、As+能与O2反应分别生成CrO+、NiO+、AsO+,而干扰离子不与O2反应,利用O2质量转移法消除了质谱干扰,选择Sc、In、Bi为内标元素校正了基体效应并防止了分析信号的漂移,实现了水产品中痕量重金属元素Cr、Ni、As、Cd、Hg、Pb的无干扰测定。采用扇贝成分分析标准物质(GBW10024)并验证了所建立方法的准确性。分析元素的检出限为0.85~4.28 ng/L,相对标准偏差≤4.65%。ICP-MS/MS的反应模式是克服质谱干扰的有效手段,可以在痕量水平上准确测定水产品中的多种重金属元素。
An analytical method for the accurate determination of multiple heavy metal elements in aquatic product by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established. For the spectral interferences caused by complex matrices in ICP-MS/MS analysis, O2 was introduced into the octopole reaction system (ORS) as the reaction gas in the MS/MS mode. The analyte Cr+, Ni+, and As+ could react with O2 to form CrO+, NiO+, and AsO+, respectively. While interference ions did not react with O2, the O2 mass shift method was used to eliminate the spectral interferences. Using Sc, In, and Bi as internal standard elements, the matrix effect was corrected and the drift of the analysis signal was prevented. The interference free determination of trace heavy metal elements Cr, Ni, As, Cd, Hg, and Pb in aquatic product was realized. The accuracy of the method proposed was evaluated by analysis of scallop composition analysis certified reference material (GBW10024). The detection limits of analytes ranged from 0.85 to 4.28 ng/L. The relative standard deviation (RSD) was ≤4.65%. Thus, ICP-MS/MS operated in the reaction mode was an effective instrumental strategy for overcoming spectral interferences, which allows the accurate determination of multiple heavy metal elements in aquatic product at trace levels.
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