摘要
目的建立干法消化和氢化物发生-双道原子荧光光谱法同时测定化妆品中砷和锑的方法。方法化妆品样品先在灰化助剂保护下进行干法消化,再加入预还原剂,优化仪器条件,选择负高压280 V,砷和锑空心阴极灯电流分别为50 mA和60 mA,用氢化物发生-双道原子荧光光谱法同时测定化妆品消解液中的砷和锑;比较不同还原剂的增敏效果;测试常见干扰离子对测定的影响;比较原子荧光光谱法同时测定和单独测定化妆品中砷和锑的统计学差异。结果采用本方法测定,砷的线性范围为0.72μg/L^10.00μg/L,r=0.9992,DL=0.15μg/L,回收率为94.4%~106.1%,精密度(RSD)为2.87%~4.36%;锑的线性范围为0.21μg/L^10.00μg/L,r=0.9999,DL=0.067μg/L,回收率为95.0%~103.5%,精密度(RSD)为1.52%~2.99%。双元素同时测定法与单元素测定法差异无统计学意义。结论测定方法简单快捷,省时省力省试剂,结果准确,满足测定要求。
Objective To establish a method for simultaneous determination of arsenic and antimony in cosmetics using dry digestion and hydride generation-atomic fluorescence spectrometry（HG-AFS）.Methods The cosmetics samples were pretreated with auxiliary ashing agents by dry digestion,then pre-reductants were added in the samples.After optimizing instruments conditions,the negative high voltage was set at 280 V,and the hollow cathode lamp current of As and Sb were set at 50 mA and 60 mA respectively.The enhanced sensitivity effect of different reductants were compared,and the influence of the common interfering ions was explored,the concentration of As and Sb in cosmetics was determined simultaneously by HG-AFS.Statistic difference was compared between the results of simultaneous determination and single（As and Sb） determination.Results The calibration curve of As was linear within the range of 0.72 μg /L - 10.00 μg /L with correlation coefficient（r） of 0.9992,and that of Sb was within the range of 0.21 μg /L - 10.00 μg /L with r = 0.9999.The detection limits were 0.15 μg /L for As and 0.067 μg /L for Sb.The recovery rates of As and Sb were 94.4% - 106.1% and 95.0% - 103.5%,respectively.The relative standard deviations（RSDs） were 2.87% - 4.36% for As and 1.52% - 2.99% for Sb.No significant difference was between the results of simultaneous determination and single（As or Sb） determination.Conclusion The method is simple,accurate and rapid enough for simultaneous determination of arsenic and antimony in cosmetics.
出处
《中国卫生检验杂志》
北大核心
2014年第11期1540-1542,共3页
Chinese Journal of Health Laboratory Technology
基金
南京市医学科技发展资金(QRX11129)
