摘要
目的 建立测定枸橼酸三乙酯中镉(Cd)、铅(Pb)、砷(As)、汞(Hg)、钴(Co)、钒(V)、镍(Ni)7 种元素杂质残留量的电感耦合等离子体-质谱法.方法 采用在线内标法,载气为氦气,等离子体模式为HMI-8,载气、雾化气、辅助气流量均为 0.8 L/min,等离子气流量为 15.0 L/min,蠕动泵转速为 0.10 r/min,雾化室温度为 2℃.结果 V,Co,Ni,As,Cd,Pb元素的质量浓度在 0～20.0 ng/mL范围内,Hg元素的质量浓度在 0～5.0 ng/mL范围内,与仪器响应值线性关系良好(r≥0.999 5,n = 7);精密度试验结果的RSD均小于 3%(n = 6);加样回收率分别为 97.58%,96.12%,96.56%,100.25%,96.63%,99.80%,106.73%,RSD 分别为 1.11%,1.29%,2.43%,1.09%,0.89%,1.26%,4.48%(n = 9).23 批样品中 7 种元素杂质含量均低于控制阈值.结论 该方法操作简便、精密度好、结果准确,可用于枸橼酸三乙酯中痕量元素杂质的含量测定.
Abstract
Objective To establish an inductively-coupled plasma-mass spectrometry(ICP-MS)method for the determination of residual quantity of seven elemental impurities[cadmium(Cd),lead(Pb),arsenic(As),mercury(Hg),cobalt(Co),vanadium(V),and nickel(Ni)]in triethyl citrate.Methods The online internal standard method was used,with helium as the carrier gas and HMI-8 plasma mode.The flow rates of the carrier gas,atomization gas,and auxiliary gas were all 0.8 L/min,the flow rate of plasma gas was 15.0 L/min,the speed of nebulizer pum was 0.10 r/min,and the temperature of atomizer chamber was 2℃.Results The linear ranges of V,Co,Ni,As,Cd,and Pb elements were 0-20.0 ng/mL,and the linear range of Hg element was 0-5.0ng/mL(r≥0.999 5,n = 7).The RSD of precision test result was lower than 3%(n = 6).The recovery rates of V,Co,Ni,As,Cd,Pb and Hg were 97.58%,96.12%,96.56%,100.25%,96.63%,99.80%,and 106.73%,with RSDs of 1.11%,1.29%,2.43%,1.09%,0.89%,1.26%,and 4.48%(n = 9),respectively.The content of seven elemental impurities in 23 batches of samples was lower than the control threshold.Conclusion This method is simple,has good precision,and accurate results,which can be used for the determination of trace elemental impurities in triethyl citrate.
维普
万方数据