目的: 建立氧化镧中元素杂质检测的ICP-MS方法,探讨用于高基体样品定量分析的ICP-MS方法开发。方法: 称取样品25 mg,置25 mL量瓶中,加硝酸1 mL和盐酸溶液0.25 mL,振摇,消解约1 h,用超纯水定容。采用Agilent 7900 ICP-MS以He模式用内标校正的标准曲线法进行样品定量测定,雾化气流速1.05 L·min-1,雾化室温度2 ℃,样品提升速度0.1 r·s-1,射频功率为1 550 W,采样深度10 mm,氦气流速5 mL·min-1,能量歧视5.0 V。依据ICH Q2(R2)和USP 2023 <233>采用加标回收率表征方法专属性,建立25种元素杂质的定量方法。以加标样品中各元素的同位素比进行专属性研究,进行待测元素的质量数选择,并完成方法验证。结果: 根据专属性考察结果Se和Ce选择82和142为检测质量数以避免干扰。方法验证结果表明24种元素杂质的线性关系良好,回收率均在70%~150%,重复性RSD≤20%,方法满足质控要求。多批次样品中检出Pb(0.152~0.201 ng·g-1)、Cd(0.007~0.010 ng·g-1)、Hg(0.156~0.250 ng·g-1)等杂质,各元素杂志的含量均低于拟定标准。结论: 本方法专属性强,准确度高,简便可行,可以为氧化镧的元素杂质控制提供技术支撑。对复杂高基体样品,加标回收率存在不足以表征方法的专属性和准确性的情况,同位素比可作为加标回收率的补充手段。
Objective: To establish an ICP-MS method for the detection of elemental impurities in lanthanum oxide and to explore the development of the ICP-MS methodology for high-matrix samples quantitative analysis. Methods: 25 mg samples were precisely weighed and placed in a 25 mL flask. 1 mL of nitric acid and 0.25 mL of hydrochloric acid solution were added, shaken, and dissolved for approximately 1 h, then fixed with ultrapure water. Quantitative samples determination were performed using Agilent 7900 ICP-MS in He mode with the standard curve method corrected by internal standard. The atomizing gas flow rate was set at 1.05 L·min-1, the atomizing chamber temperature was maintained at 2 ℃, the sample aspiration rate was 0.1 r·s-1, the RF power was 1 550 W, and the sampling depth was 10 mm. The helium flow rate was 5 mL·min-1, and the energy discrimination was 5.0 V. Based on ICH Q2 (R2) and USP 2023 <233>, a quantitative method for 25 elemental impurities was established by utilizing the recovery rate of the method. The isotope ratio of each element in the sample was investigated, the mass number of the element to be measured was selected, and the method was verified. Results: Based on the specific outcomes of Se and Ce, 82 and 142 were chosen as the detection mass numbers to evade interference. The results demonstrated that the linear relationships of the 24 elemental impurities were excellent, the recoveries ranged from 70% to 150%, the repeatability RSDs were less than 20%, and the method satisfied the quality control requirements. Impurities such as Pb (0.152-0.201 ng·g-1), Cd (0.007-0.010 ng·g-1), Hg (0.156-0.250 ng·g-1) were detected in numerous batches of samples, and the contents of each element were lower than the proposed standard. Conclusion: The method is specific, accurate, simple, and feasible, and can furnish technical support for the elemental impurity control of lanthanum oxide. For complex and high-matrix samples, the recovery rate of standard addition is inadequate to characterize the specificity and accuracy of the method, and the isotope ratio can be utilized as a supplement to the recovery rate of standard addition.
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