电感耦合等离子体-质谱法测定益肾壮骨丸中6种重金属含量

目的建立测定益肾壮骨丸中6种重金属元素含量的电感耦合等离子体-质谱(ICP-MS)法。方法射频功率为1 550 W,冷却气、辅助气流速分别为14.0,0.8 L/min,采样锥和截取锥为镍锥,重复次数为3次,采样模式为KED模式,蠕动泵转速为40 r/min,并加入内标元素校正响应信号波动。结果铅(Pb)、砷(As)、汞(Hg)、镉(Cd)、铜(Cu)、铬(Cr)元素质量浓度分别在0～20 ng/mL,0～20 ng/mL,0～2 ng/mL,0～10 ng/mL,0～500 ng/mL,0～100 ng/mL范围内与各待测元素/内标元素仪器信号强度线性关系良好(r> 0.995);检测限分别为0.029,0.005,0.016,0.001,0.022,0.022 ng/mL;多数元素精密度、重复性试验的RSD小于2.0%;平均加样回收率分别为88.03%,96.64%,83.75%,91.51%,95.63%,94.49%,RSD分别为6.99%,5.41%,3.68%,2.70%,1.87%,3.31%(n=6)。结论该方法灵敏、准确,可用于益肾壮骨丸中重金属元素Pb,As,...

Content Determination of Six Heavy Metals in Yishen Zhuanggu Pills by ICP-MS

Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the content determination of six heavy metals in Yishen Zhuanggu Pills.Methods The radio frequency(RF)power was 1550 W,the flow rates of cooling gas and auxiliary gas were 14.0 L/min and 0.8 L/min respectively,the sampling cone and interception cone were nickel cone,the repetition times were three times,the sampling mode was KED mode,the peristaltic pump speed was 40 r/min,and internal standard elements were added to correct the response signal fluctuation.Results The mass concentrations of lead(Pb),arsenic(As),mercury(Hg),cadmium(Cd),copper(Cu)and chromium(Cr)showed a good linear relationship with the instrument signal intensity of each element to be tested/internal standard element in the range of 0-20 ng/mL,0-20 ng/mL,0-2 ng/mL,0-10 ng/mL,0-500 ng/mL,0-100 ng/mL(r>0.995),respectively.The limits of detection(LOD)were 0.029,0.005,0.016,0.001,0.022 and 0.022 ng/mL,respectively.The RSDs of precision and repeatability tests of most elements were less than 2.0%.The average recoveries of Pb,As,Hg,Cd,Cu and Cr were 88.03%,96.64%,83.75%,91.51%,95.63%and 94.49%with RSDs of 6.99%,5.41%,3.68%,2.70%,1.87%and 3.31%(n=6),respectively.Conclusion The method is sensitive and accurate,it can be used for the determination of heavy metal elements Pb,As,Hg,Cd,Cu and Cr in Yishen Zhuanggu Pills,and it is helpful to evaluate the safety of the products in all production links.