CAJ | 학술논문

应用液相色谱-等离子质谱联用的方法分析食品样品中的主要有机砷(一甲基砷和二甲基砷)和无机砷(三价砷和五价砷). 采用50%(体积分数)甲醇水溶液作为萃取剂,将食品样品进行预处理,再以5 mmol/L四丁氢铵,2 mmol/L丙二酸和5%(体积分数)甲醇水溶液作为流动相(pH 5.9),C18色谱柱(150 mm×4 mm i.d., 5 μm)将样品萃取液进行液相色谱分离,最后进入等离子质谱仪定性分析. 经测定发现,新鲜蔬菜和水果样品中主要含有的无机砷为三价砷和五价砷,有机砷为二甲基砷.一甲基砷在个别样品中也有发现.该法的检出限分别为:三价砷0.2 μg/kg,五价砷0.6μg/kg和二甲基砷0.3 μg/kg.
응용액상색보-등리자질보련용적방법분석식품양품중적주요유궤신(일갑기신화이갑기신)화무궤신(삼개신화오개신). 채용50%(체적분수)갑순수용액작위췌취제,장식품양품진행예처리,재이5 mmol/L사정경안,2 mmol/L병이산화5%(체적분수)갑순수용액작위류동상(pH 5.9),C18색보주(150 mm×4 mm i.d., 5 μm)장양품췌취액진행액상색보분리,최후진입등리자질보의정성분석. 경측정발현,신선소채화수과양품중주요함유적무궤신위삼개신화오개신,유궤신위이갑기신.일갑기신재개별양품중야유발현.해법적검출한분별위:삼개신0.2 μg/kg,오개신0.6μg/kg화이갑기신0.3 μg/kg.
The speciation of arsenic in food samples was analyzed. The methods used for sample preparation include: the extraction of arsenic from food samples using a 1∶1 (v/v) methanol/water, and high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) determination of the speciation of arsenic in food samples. A C18 column was used to separate the arsenic species. The mobile phase consists of 5 mmol/L tetrabutylammonium hydride, 2 mmol/L malonic acid and 5% (v/v) methanol solution with the pH adjusted to 5.9. The mobile phase flow rate was 1.2 mL/min. The chemical species of arsenic present in the foodstuffs were found mainly As (Ⅲ), As (Ⅴ), dimethylarsinic (Ⅴ) (DMA (Ⅴ)). Detection limit was based on signal to noise ratio of 3. As to apple samples, the detection limits were 0.2, 0.6 and 0.3 μg/kg for As (Ⅲ), As (Ⅴ) and DMA (Ⅴ), respectively. The concentrations of arsenic in raw apple samples were calculated.