微量直接进样-二元泵联用ICP-MS分析大米蛋白中痕量铅  

The study on determination of trace lead in rice protein samples by ICP-MS coupled with direct injection-binary pump system

作　　者：方勇[1] 陈悦[1] 鞠兴荣[1] 文良[2] 薛梅[1] 马宁[1] 赵立艳[3] 胡秋辉[1,3] 

机构地区：[1]南京财经大学食品科学与工程学院,江苏省现代粮食流通与安全协同创新中心,南京210023 [2]深圳出入境检验检疫局,深圳518045 [3]南京农业大学食品科技学院,南京210095

出　　处：《分析试验室》2015年第2期151-154,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(31471680);国家粮食公益性行业科研专项(201313007);江苏省自然科学基金(BK2011833);江苏省高校自然科学基金项目(10KJA550011);江苏省青蓝工程和江苏省优势学科建设工程资助

摘　　要：建立了微量直接进样—二元泵联用ICP-MS分析大米蛋白样品中痕量铅的方法。将酶解后的大米蛋白液离心,取上清液过0.45μm膜直接进样。优化分析条件：流动相为体积分数2%HNO3/甲醇（99：1,V/V）,流速0.5 m L/min,进样量50μL。在0-50μg/L范围内线性相关系数为0.9998,方法检出限为5.37 ng/L,加标样品的回收率在93.2%-97.4%之间,RSD为0.96%-4.1%（n=9）。方法可作为大米蛋白中痕量铅的批量分析方法。To determine the content of trace lead in rice protein,the method of ICP-MS coupled with direct micro injection-binary pump system was established. The protein hydrolyzates were centrifuged,passed through0. 45 μm membrane,and then directly sampled by the injection system. Under the optimal conditions,2% nitric acid / methanol（ V / V = 99： 1） was used as the mobile phase with a flow rate of 0. 5 m L / min,and an injection volume of 50 μL. The linear range was 0 - 50 μg / L with correlation coefficient above 0. 9998,while the limit of determination was 5. 37 ng / L,recoveries of spiked samples were from 93. 2% to 97. 4%,and the RSDs（ n = 9）were from 0. 96% to 4. 1%. The protein hydrolyzates showed a good stability in the mobile phase,and they could be directly injected without digestion. Therefore,the method could be considered for batch analysis of trace lead in rice protein samples with little injection volume and short analysis time.

关 键 词：直接进样 电感耦合等离子体质谱(ICP-MS) 铅 大米蛋白 

分 类 号：O657.63[理学—分析化学]