应用ICP-MS同时测定裸花紫珠干浸膏中6种重金属元素的含量

Simultaneous determination of 6 kinds of heavy metal in Callicarpa nudiflora dry extract by ICP-MS

目的建立电感耦合等离子体质谱法(ICP-MS)同时测定裸花紫珠干浸膏中6种重金属元素铬(Cr)、铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、镍(Ni)的含量。方法采用微波消解法处理样品,以锗(Ge)、铟(In)、铋(Bi)作为内标,紫菜标准物质作为质控,通过ICP-MS同时测定6种重金属元素。结果 6种重金属元素的线性范围为0~40 ng/m L,相关系数在0.998 2~0.999 9之间;定量限(LOQ)在0.004 9~0.065 9 ng/m L;精密度、重复性和稳定性良好,相对标准偏差(RSD)均<2.0%;低中高3个水平的加样回收率在90.0%~101.6%之间。依据本方法检验了3批样品,铬(Cr)的含量为0.198 3~0.2132 mg/kg、铅(Pb)的含量为0.498 7~0.706 5 mg/kg、镉(Cd)的含量为0.032 5~0.061 3 mg/kg、汞(Hg)的含量为0.006 4~0.008 4 mg/kg、砷(As)的含量为0.148 6~0.286 3 mg/kg、镍(Ni)的含量为0.685 7~0.710 1 mg/kg。结论该方法操作简便、结果准确、重复性好,可用于同时测定裸花紫珠干浸膏中6种重金属元素的含量。

Objective To establish a method for simultaneous determination of 6 kinds of heavy metal（Cr, Pb, Cd, Hg,As, Ni） in Callicarpa nudiflora dry extract by ICP-MS. Methods The samples were conducted pretreatment by microwavedigestion instrument. Ge, In, and Bi were applied as internal standard elements and nori was applied as the standard referencematerial of determining the contents of six kinds of heavy metal by ICP-MS simultaneously.Results The calibration curves ofthe six kinds of heavy metal were in the range of 0-40 ng/m L, with the correlation coefficients between 0.998 2 and 0.999 9.The limit of quantitation（LOQ） of the method was in the range of 0.004 9-0.065 9 ng/m L; the precision,reproducibility andstability of the method were in good condition, and their relative standard deviations（RSD） were less than 2.0%; the recoveriesof three different concentrations were in the range of 90.0%-101.6%. Three batches of samples were detected, and the resultsof the content were：Cr was ranged from 0.198 3 to 0.213 2 mg/kg, Pb was ranged from 0.498 7 to 0.706 5 mg/kg, Cd was rangedfrom 0.032 5 to 0.061 3 mg/kg, Hg was ranged from 0.006 4 to 0.008 4 mg/kg, As was ranged from 0.148 6 to 0.286 3 mg/kg,and Ni was ranged from 0.685 7 to 0.710 1 mg/kg. Conclusion The method is simple and accurate, and it also has goodreproducibility. The method could be used for simultaneous determination of the contents of six kinds of heavy metal in Callicarpa nudiflora dry extract.