摘要
目的 建立测定注射用芝麻油中 10 种无机元素含量的电感耦合等离子体质谱(ICP-MS)法.方法 采用微波消解法前处理样品,采用ICP-MS内标标准曲线法检测各元素含量,射频功率为 1 500 W,雾化室温度为 2℃,采用氦碰撞模式,载气(氩气)流速为0.8 L/min.结果 铅、镉、砷、汞、钴、钒、镍、锂、锑、铜质量浓度分别在 1.25～12.5 ng/mL、0.50～5.0 ng/mL、4.00～40.0 ng/mL、0.75～7.5 ng/mL、1.25～12.5 ng/mL、2.50～25.0 ng/mL、5.00～50.0 ng/mL、62.50～625.0 ng/mL、22.50～225.0 ng/mL、75.00～750.0 ng/mL范围内与各元素和内标仪器响应值比值线性关系良好(r>0.990 0),检测限为 0.000 2～0.042 0 μg/g,定量限为 0.075～7.5 μg/g;精密度、重复性试验结果的RSD均小于 10%;平均加样回收率为 78.64%～110.39%,RSD为 1.40%～6.41%(n= 9).结论 所建立的方法灵敏,结果准确可靠,可用于注射用芝麻油中 10 种无机元素含量的测定.
Abstract
Objective To establish the inductively coupled plasma-mass spectrometry(ICP-MS)method for determining the contents of 10 inorganic elements in Sesame Oil for Injection.Methods The samples were pretreated by the microwave digestion method,and the contents of inorganic elements were detected by the ICP-MS internal standard curve method.The radio frequency power was 1 500 W,the nebulizer temperature was 2℃,the helium collision mode was adopted,and the carrier gas(argon)flow rate was 0.8 L/min.Results The linear ranges of lead,cadmium,arsenic,mercury,cobalt,vanadium,nickel,lithium,antimony and copper were 1.25-12.5 ng/mL,0.50-5.0 ng/mL,4.00-40.0 ng/mL,0.75-7.5 ng/mL,1.25-12.5 ng/mL,2.50-25.0 ng/mL,5.00-50.0 ng/mL,62.50-625.0 ng/mL,22.50-225.0 ng/mL,75.00-750.0 ng/mL respectively(r>0.990 0).The limit of detection(LOD)was in the range of 0.000 2 to 0.042 0 μg/g,and the limit of quantitation(LOQ)was in the range of 0.075 to 7.5 μg/g.The RSDs of precision and repeatability tests were lower than 10%.The average recovery rates of the above 10 inorganic elements were in the range of 78.64%to 110.39%,with the RSDsof 1.40%to 6.41%(n = 9).Conclusion The established method is sensitive,accurate and reliable,which can be used for the determination of 10 inorganic elements in Sesame Oil for Injection.
国家科技期刊平台
NSTL
维普
万方数据