摘要
为减少生物样品在消解过程中Se的挥发损失,增加测定灵敏度,提高精密度,消除质谱法测定过程中的干扰,保证测定准确度,采用微波密闭消解-乙醇增敏-串联质谱(ICP-MS/MS)法测定生物样品中的硒。生物样品经微波密闭消解后,在MS/MS模式下,在线引入含有7%乙醇的Rh内标溶液,用乙醇增敏,提高仪器信号灵敏度,通过Se^(+)与O_(2)反应形成SeO^(+),实现质量转移消除了Se的质谱干扰。对同位素的选择、干扰因素分析和消除、乙醇的增敏效果、仪器条件等进行了讨论。结果表明,方法检出限为0.004μg/g,以国家一级标准物质进行精密度和准确度实验,相对标准偏差为2.5%~6.6%,测定平均值和标准物质认定值的ΔLogc在±0.05以内,相对误差RE在±10%以内,测定值与标准值相吻合。方法在富硒区域调查、富硒农产品及食品检测等工作中具有较好应用前景。
In order to reduce the volatile loss of sein the digestion process,increase the determination sensitivity,improve the precision,eliminate the interference in the determination process of mass spectrometry,and ensure the accuracy,microwave closed digestion-ethanol sensitization-tandem mass spectrometry(ICP-MS/MS)method was adopted for Se determination of biological samples.After the biological samples were digested by microwave,the Rh internal standard solution containing 7%ethanol was introduced online in MS/MS mode,and the sensitivity of the instrument signal was improved by ethanol sensitization.SeO^(+) was formed by Se+reaction with O_(2),which realized mass transfer and eliminated the mass spectrum interference of Se.The selection of isotope,analysis and elimination of interference factors,sensitization effect of ethanol and instrument conditions were discussed.The detection limit of the method was 0.004μg/g.The relative standard deviations of precision and accuracy experiments were 2.5%-6.6%with the national standard material.TheΔLog c and RE were within±0.05 and±10%respectively,and the measured values were consistent with standard values.This method has a good application prospect in selenium-rich area survey,selenium-rich agricultural products and food detection.
作者
张啟云
张武萍
ZHANG Qiyun;ZHANG Wuping(Qinghai Province Geological and Mineral Testing and Application Center,Xining,Qinghai 810021,China)
出处
《中国无机分析化学》
CAS
北大核心
2023年第10期1149-1153,共5页
Chinese Journal of Inorganic Analytical Chemistry
关键词
微波密闭消解
乙醇增敏
串联质谱
生物样品
硒
microwave airtight digestion
ethanol sensitizes
ICP-MS/MS
biological samples
selenium
