微波消解/ICP-MS法测定人体肋骨中痕量镧系元素

Application of microwave dissolution and inductively coupled plasma-MS spectrometry for determination of ultra-trace level of lanthanides in human rib

建立了用HNO3 微波消解体系 ,以铑为内标 ,电感耦合等离子体质谱法 (ICP MS)法直接测定肋骨中痕量镧系元素镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥的新方法。方法快速、灵敏、准确 ,检出限分别在 0 0 0 0 7～ 0 0 0 5 μg L之间 ,线性良好 ,线性相关系数r均≥ 0 997;精密度良好 ,RSD <3% ;回收率在93 7%～ 115 4%之间。内标元素Rh可补偿基体效应 ,干扰校正系数法可校正基体中钡氧化物 氢氧化物的质谱干扰。用人发标准物质GBW0 76 0 1及小麦粉标准物质GBW0 85 0 3质控 ,实际成人肋骨样品测定 。

A new method for the determination of ultra-trace level of lanthanides such as La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm Yb and Lu in human rib is explored. Closed-vessel microwave digestion with concentrated HNO 3 is used for the sample preparation and the digested analyte is directly analyzed by ICP-MS. The method is sensitive and accurate and, is efficient for the determination of the fourteen lanthanides listed above. Detection limit for various elements ranges from 0.0007μg/L to 0.005μg/L. Calibration plots exhibit good linearity with high linear correlation coefficient r≥0.997. Recoveries of spiked samples ranges from 93.7% to 115.4%. Precision is <3%RSD. Rhodium is used as the internal standard to compensate the signal suppression caused by the sample matrix. Isobaric overlap of polyatomic ions caused by matrix oxide/hydroxide of barium is corrected by interference correction factor. Two standard reference materials, namely “Human Hair GBW07601' and “Wheat Flour GBW08503' are used for quality control of the analyzed samples.