ICP-MS法测定决明子中18种重金属及有害元素

Determination of Eighteen Heavy Metals and Hazardous Elements in Cassiae semen by Using ICP-MS Method

该试验旨在建立决明子中重金属及有害元素残留量的测定方法,为进一步提高决明子的药材质量,保证其用药安全提供科学依据。采用压力罐消解法对样品进行消解,利用电感耦合等离子体质谱(ICP-MS)法测定决明子样品中铅、镉、砷、汞、铜、锂、铍、钒、铬、锰、钴、镍、钼、锡、锑、钡、镝、铊共18种重金属及有害元素含量,并对检测手段进行方法学考察。结果表明,Cr,Mn,Ni,Cu和Ba线性范围为1~500 ng/mL,Li,Be,V,Co,As,Mo,Cd,Sn,Sb,Dy,Tl,Pb和Hg线性范围为0.1~50 ng/mL,标准曲线的线性相关系数均大于0.99,精密度考察与稳定性考察S_(RSD) (相对标准偏差)均小于4%,重复性考察S_(RSD)在1.65%~6.79%之间,平均加样回收率在94.6%~108.5%之间,S_(RSD)均小于10%。试验采用的方法简单、准确、重复性好,可用于准确测定决明子中18种重金属及有害元素的含量,为决明子提供更为全面的质量控制方法。

The study was in order to establish a method for the determination of heavy metals and hazardous elements in Cassiae semen,so as to provide a reference for risk evaluation,standard improvement and quality supervision for Cassiae semen.About 18 heavy metals and hazardous elements of Pb,Cd,As,Hg,Cu,Li,Be,V,Cr,Mn,Co,Ni,Mo,Sn,Sb,Ba,Dy and Tl in Cassiae semen were determined by using high pressure digestion and ICP-MS.The methods were validated.The results showed that the linear range of Cr,Mn,Ni,Cu,Ba was 1-500 ng/mL,and that of Li,Be,V,Co,As,Mo,Cd,Sn,Sb,Dy,Tl,Pb and Hg was 0.1-50 ng/mL.The standard curves were linear and the linear correlation coefficients were greater than 0.99.The relative standard deviation S_(RSD)(precision and stability) was less than 4%,and the repeatability S_(RSD) was 1.65%-6.79%.The recovery was 94.6%-108.5%,and S_(RSD) were all lower than 10%.The established method was simple,accuracy,reproducible.It could be used for the determination of 18 heavy metals and hazardous elements in Cassiae semen,so as to provide more comprehensive quality control methods for Cassiae semen.