微波消解—ICP-OES/ICP-MS法测定桂花中46种元素

摘要

Objective To established a method to determine 46 elements in Osmanthus fragrans by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS).Methods HNO3-H2O2 was used to decompose Osmanthus fragrans with microwave digestion.ICP-OES was applied to determine the elements of Na,Mg,Al,P,S,K,Caand Fe,the others (Ag,As,Ba,Cd,Co,Cr,Cs,Cu,Hg,Li,Mn,Mo,Ni,Pb,Rb,Se,Sn,Sr,Th,Ti,TI,V,Zn and 15 kinds of rare earth elements) were determined by ICP-MS.Results Determination limits of ICP-OES were in the range of 0.68～ 18.10 μg/L while ICP-MS were in the range of 0.001 ～0.093 μg/L.The relative standard deviations (RSDs) were in the range of 0.84％ ～8.42％,and the recoveries of 46 trace elements were in the range of 87.2％～ 113.6％.The proposed method was applied in the analysis of reference material bush branch and leaf [GBW07603 (GSV-2)],giving results in consistency with the certified values.The analytical results showed that large amounts of elements were embodied in Osmanthus fragrans.There were 13 kinds of elements with their contents in Osmanthus fragrans more than 10 mg/kg,the contents of beneficial elements Na,Mg,P,S,K,Ca,Fe and Zn and harmful elements Al,Ni,Ba and Pb in Osmanthus fragrans were high.Conclusion This analysis method was simple,rapid,accurate and could be applied for simultaneous determination of elements in Osmanthus fragrans.%为建立采用电感耦合等离子体发射光谱(ICP-OES)/电感耦合等离子体质谱(ICP-MS)测定桂花中46种元素的方法.将样品经HNO3-H2O2微波消解后,以ICP-OES测定桂花中Na、Mg、A1、P、S、K、Ca和Fe,ICP-MS测定桂花中Ag、As、Ba、Cd、Co、Cr、Cs、Cu、Hg、Li、Mn、Mo、Ni、Pb、Rb、Se、Sn、Sr、Th、Ti、T1、V、Zn和15种稀土元素.结果表明:ICP-OES检出限为0.68～18.10 μg/L,ICP-MS检出限为0.001～0.093 μg/L.方法精密度(RSD)为0.84％～8.42％,回收率为87.2％～113.6％.国家标准物质灌木枝叶[GBW07603(GSV-2)]的检测结果与参考值基本一致.桂花测定结果表明桂花中富含多种微量元素,其中含量在10 mg/kg以上的有13种.测定的元素中含量较高的有益元素为Na、Mg、P、S、K、Ca、Fe和Zn,而含量较高的有害元素有Al、Ni、Ba和Pb.该方法具有快速、简便、准确等优点,适用于桂花中多种元素的同时测定.