ICP-MS同时测定当归中12种人体必需微量元素及5种重金属元素的含量

Simultaneous Determination of 12 Essential Trace Elements and 5 Heavy Metal Elements in Angelica Sinensis(Oliv.) Diels by ICP-MS

建立一种检出限低、灵敏度高、线性范围宽、精密度高且可实现多种元素同时测定的分析方法,检测3个不同批次当归中17种微量元素的含量,包括12种人体必需微量元素(锰Mn、铬Cr、锶Sr、锌Zn、铷Rb、硼B、镍Ni、钒V、锡Sn、锰Mo、硒Se、钴Co)以及5种重金属元素(铜Cu、砷As、铅Pb、镉Cd、汞Hg),填补该药用植物ICP-MS法测定其微量元素的空白,为其质量控制及药效物质基础的研究提供科学依据。试验采用电感耦合等离子体质谱法测定,所测样品以HNO_(3-)H_2O_2体系为湿法消解系统,以铟、铑为内标,标准曲线法计算各元素的含量。方法学验证结果显示,17种微量元素在0.05～150.00μg/L范围内线性关系良好,相关系数r均大于0.999,各元素的检出限为0.001 8～0.120 3μg/g,精密度、重复性、稳定性试验的RSD分别不大于3.95%、2.93%、3.42%,加样回收率为96.67%～100.48%。测得Mn、Cr、Sr、Zn、Rb、B、Ni、V、Sn、Mo、Se、Co、Cu、As、Pb、Cd、Hg各元素质量分数分别为35.550μg/g、15.930μg/g、20.100μg/g、25.700μg/g、11.170μg/g、32.600μg/g、6.140μg/g、3.292μg/g、1.173μg/g、0.414μg/g、1.452μg/g、0.456μg/g、13.170μg/g、0.696μg/g、0.621μg/g、0.034μg/g、0.091μg/g。本快速测定方法精密度高、重复性和稳定性良好、结果准确可靠。当归中含有较丰富的Mn、B、Zn、Sr、Cr、Rb等人体必需微量元素,5种重金属元素的含量均未超标。

An analytical method for simultaneous determination of multiple elements with low detection limit, high sensitivity, wide linear range and high precision was established to detect the contents of 17 trace elements in three different batches of Angelica sinensis. These elements include 12 essential trace elements of human body, namely Mn,Cr,Sr,Zn,Rb,B,Ni,V,Sn,Mo,Se,Co, and 5 heavy metal elements including Cu, As, Pb, Cd and Hg. To fill in the blank of the determination of trace elements by ICP-MS method, and to provide scientific data for the quality control and the research on the basis of medicinal materials.Adopting the method of electric heating digestion, the samples were digested respectively with the mixed HNO3-H2O2 system, the contents of trace elements were determined by ICP-MS. In addition, In and Rh were regarded as internal standard, and the contents of trace elements were calculated by standard curve method.The methodological study result showed that the linear relationship of these 17 elements in the range of 0.05-150.00μg/g abstained good results, and the linear correlation coefficients were greater than 0.999, the detection limits were in the range of 0.001 8-0.120 3μg/g,the RSD of precision, repeatability and stability experiments were not more than 3.95%, 2.93% and 3.42%,the recoveries were 96.67%-100.48%. The contents of Mn,Cr,Sr,Zn,Rb,B,Ni,V,Sn,Mo,Se,Co,Cu,As,Pb,Cd,Hg were 35.550μg/g,15.930μg/g,20.100μg/g,25.700μg/g, 11.170μg/g,32.600μg/g,6.140μg/g,3.292μg/g,1.173μg/g,0.414μg/g,1.452μg/g, 0.456μg/g, 13.170μg/g, 0.696μg/g, 0.621μg/g,0.034μg/g,0.091μg/g, respectively. This method was proved to be high precision, repeatability and stability, and accurate. Our results indicate that A.sinensis contains abundant human essential trace elements such as Mn, B, Zn, Sr, Cr, Rb, etc., and the contents of five heavy metals do not exceed the criterion.