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目的建立加速溶剂萃取(PLE)与高效液相色谱-电感耦合等离子体质谱(HPLC-ICP MS)联用测定海产品中砷形态的方法,为食品安全风险监测提供参考方法。方法以50%甲醇-水为溶剂,采用快速溶剂萃取仪提取各形态的砷;利用阴离子交换柱分离,以O2为动态反应气消除质谱干扰,实现了As B、As(Ⅲ)、DMA、MMA、As(Ⅴ)5种形态砷的分离测定。结果 5种砷浓度在2.5μg/L~25μg/L时线性相关系数均≥0.999 0,检出限为0.1μg/L~0.2μg/L,相对标准偏差<3.5%。实际样品加标回收率在80.1%~104.0%。结论方法具有快捷、准确、灵敏等优点,可分别用于无机砷、有机砷的测定,并可最大程度保留食品中砷的原始形态,便于进行形态分布研究。
Objective To establish a method for determination of arsenic in seafood by accelerated solvent extraction (PLE) and high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS), and provide a reference method for the monitoring of food safety risk. Methods As (Ⅲ), DMA, MMA and As (Ⅲ) were obtained by the rapid solvent extraction using 50% methanol-water as solvent and the separation by anion exchange column. , As (Ⅴ) five kinds of forms of arsenic separation and determination. Results The linear correlation coefficients of five arsenic concentrations from 2.5μg / L to 25μg / L were all ≥ 0.9999 with the detection limits of 0.1μg / L ~ 0.2μg / L with relative standard deviations of 3.5%. The actual sample spike recovery was 80.1% ~ 104.0%. Conclusion The method is rapid, accurate and sensitive. It can be used for the determination of inorganic arsenic and organic arsenic, respectively, and can preserve the original form of arsenic in food to the maximum extent and facilitate the study of morphological distribution.