摘要
建立快速石墨消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定海菜中13种元素含量的方法.通过单因素试验优选海菜快速石墨消解最佳条件,以^45 Sc、^72 Ge、^115 In、^209 Bi为内标,用ICP-MS同时测定海菜中13种元素.海菜快速石墨消解最佳条件为,HNO32.0 mL,H2 O21.0 mL,温度120℃,时间20 min.Na、Mg、K、Ca在0~10 mg/L,Mn、Ni、Cu、Zn、As、Sr、Cd、Ba、Pb在0~0.3 mg/L线性良好,相关系数均≥0.9995.13种元素的检出限为0.0006~0.6701 mg/kg,定量限为0.0020~2.2338 mg/kg,相对标准偏差为0.34%~5.31%,回收率为87.6%~108.5%.采用该法处理国家标准物质螺旋藻(GBW10025),测定结果在参考值范围内.该法简单、快速、准确、可靠,可用于植物样品中多元素分析的样品前处理和测定.
A method for determining Na,Mg,K,Ca,Mn,Ni,Cu,Zn,As,Sr,Cd,Ba and Pb in Ottelia acuminate by ICP-MS combined with rapid graphite digestion was established in this study. The rapid graphite digestion condition was optimized single factor test,^45 Sc,^72 Ge,^115 In and ^209 Bi were used as internal standard elements,and the content of each element was simultaneously determined by ICP-MS. The optimum condition of rapid graphite digestion was as follows: used 2.0 mL nitric acid and 1.0 mL hydrogen peroxide,and digested at 120 ℃ for 20 min. The linear ranges of Na,Mg,K and Ca were 0-10 mg/L,of Mn,Ni,Cu,Zn,As,Sr,Cd,Ba and Pb were 0-0.3 mg/L,and the correlation coefficients were all higher than 0.999 5. The detection limits and quantification limits of the elements were in the range of 0.000 6-0.670 1 mg/kg and 0.002 0-2.233 8 mg/kg,respectively. The relative standard deviation of the method was between 0.34% and 5.31%,and the recovery rate was 87.6%-108.5%. The contents of these 13 elements in national standard material (GBW10025) were in the range of reference values by applying the established method. In conclusion,this method is simple,fast,accurate and reliable,which can be used for analyzing multielement in plant samples.
作者
杨春花
毕健梁
周美丽
杨伟
范晓旭
YANG Chunhua;BI Jianliang;ZHOU Meili;YANG Wei;FAN Xiaoxu(Food Inspection and Testing Institute of Dali,Dali 671000,China;Comprehensive Inspection and Testing Institute ofHeqing,Heqing 671500,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2019年第16期281-285,共5页
Food and Fermentation Industries
关键词
快速石墨消解
电感耦合等离子体质谱
海菜
无机元素
rapid graphite digestion
inductively coupled plasma mass spectrometry (ICP-MS)
Ottelia acuminate
inorganic elements