微波消解-电感耦合等离子体质谱法测定虾皮中28种元素

Determination of 28 elements in dried small shrimps by microwave digestion with inductively coupled plasma mass spectrometry

中文关键词:  虾皮  元素  电感耦合等离子体质谱法

英文关键词:dried small shrimps  elements  inductively coupled plasma mass spectrometry

中文摘要:

      目的 建立电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)测定虾皮中K、Na、Ca、Mg、Fe、Mn、Cu、Zn、P、Li、Al、V、Cr、Co、Ni、As、Rb、Sr、Se、Mo、Ag、Cd、Pb、Ba、Ga、Cs、Tl、Bi 28种元素含量的分析方法。方法 采用硝酸-过氧化氢消解体系, 通过在线加入Ge、Rh、Re内标进行基体效应校正, 碰撞反应池模式(kinetic energy discrimination, KED)消除多原子离子干扰, 以国家标准物质大虾(GBW 10050)为研究对象, 验证方法准确度。结果 方法检出限为0.001～0.681 mg/kg, 相对标准偏差(relative standard deviations, RSD)为0.6%～8.2%, 各元素标准曲线线性关系良好, 相关系数r2大于0.999, 样品回收率为87.4%～110.0%。虾皮中常量元素K、Na、Ca、Mg等含量较高, Pb、Cd、Cr等重金属元素含量较低, Al、As需根据其存在形态评估可能存在的健康安全风险。结论 该方法准确高效, 灵敏度高, 可应用于虾皮样品分析。

英文摘要:

      Objective To establish a method for determination of 28 kinds of elements including K, Na, Ca, Mg, Fe, Mn, Cu, Zn, P, Li, Al, V, Cr, Co, Ni, As, Rb, Sr, Se, Mo, Ag, Cd, Pb, Ba, Ga, Cs, Tl, Bi in dried small shrimps by microwave digestion with inductively coupled plasma mass spectrometry (ICP-MS). Methods Nitric acid and hydrogen peroxide was used to digest samples, internal standard elements Ge, Rh and Re were added online to correct matrix effect, and kinetic energy discrimination (KED) was selected to eliminate polyatomic ion interference. Prawn reference material (GBW 10050) was used to verify the accuracy of the method. Results The limits of detection were 0.001?0.681 mg/kg, the relative standard deviations (RSDs) were 0.6%?8.2%, the linearity of elements standard curves was good and the correlation coefficients were more than 0.999, and the recoveries were in the range of 87.4%?110.0%. The content of macro-elements of K, Na, Ca, Mg was high, and the content of heavy metals of Pb, Cd, Cr was low. Health and safety risks of Al and As should be assessed based on the speciation. Conclusion This method is accurate, efficient and sensitive, and can meet the requirements for the determination of elements in dried small shrimps.