电感耦合等离子体发射光谱/质谱法测定蚝油中15种元素

Determination of 15 elements in oyster sauce by inductively coupled plasmaoptical emission/mass spectrometry

建立了电感耦合等离子体发射光谱/质谱法(inductively coupled plasma optical emission spectrometry/inductively coupled plasma mass spectrometry,ICP-OES/ICP-MS)测定蚝油中K、Na、Ca、Mg、P、Fe、Mn、Cu、Zn、Al、As、Pb、Cd、Cr、Se 15种元素含量的分析方法,评估其营养价值和可能存在的健康安全风险。采用HNO_(3)-H_(2)O_(2)消解体系,通过分析线的筛选消除ICP-OES的光谱干扰,通过在线加入Ge、Rh、Re内标结合动能歧视效应(kinetic energy discrimination,KED)消除ICP-MS的基体效应和质谱干扰,以国家标准物质扇贝(GBW 10024)为研究对象,验证方法准确度。ICP-OES各元素的检出限为0.125~0.987 mg/kg,平均回收率为89.3%~103.5%,相对标准偏差(relative standard deviations,RSD)为0.2%~3.7%;ICP-MS各元素的检出限为0.001~0.014 mg/kg,平均回收率为87.2%~107.8%,RSD为0.2%~2.7%。标准曲线线性关系良好(R^(2)>0.999)。蚝油中K、Na、Ca、Mg等常量元素含量较高,As、Pb、Cd、Cr等重金属元素含量较低。该方法准确高效,灵敏度高,可应用于蚝油样品分析。

A method for determination of 15 kinds of elements of K,Na,Ca,Mg,P,Fe,Mn,Cu,Zn,Al,As,Pb,Cd,Cr,Se in oyster sauce by inductively coupled plasma optical emission spectrometry/inductively coupled plasma mass spectrometry(ICP-OES/ICP-MS)was established,and the nutritive value and possible risks of health and safety were assessed.The samples were digested by nitric acid and hydrogen peroxide.The spectral interference of ICP-OES was eliminated by selecting different analysis lines,and the matrix effect of ICP-MS was diminished by adding internal standard elements of Ge,Rh,and Re online,and the mass spectral interference was diminished by kinetic energy discrimination(KED).In addition,scallop reference material(GBW 10024)was used to verify the accuracy of the method.The results showed that the detection limits of ICP-OES were 0.125-0.987 mg/kg with 89.3%-103.5%the average recoveries,and the relative standard deviations(RSD)were 0.2%-3.7%.While the detection limits of ICP-MS were 0.001-0.014 mg/kg,the average recoveries were 87.2%-107.8%and the RSD was 0.2%-2.7%.The linear relationship of standard curves was good(R^(2)>0.999).The contents of macro-elements of K,Na,Ca,Mg in the oyster sauce were high,while heavy metals of As,Pb,Cd,Cr were low.This method is accurate,efficient and sensitive.It can meet the requirements for the determination of elements in oyster sauce.