电感耦合等离子质谱法测定豆制品中铝含量的不确定度评定及方法改进

本文采用微波消解-电感耦合等离子体质谱法（ICP-MS）测定豆制品中铝的含量，对测定过程中可能引入的不确定度进行分析和评定。根据CNAS-CL01-G003:2019对测定不确定度的有关要求，建立了不确定度评定的数学模型，分析不确定度的主要来源，并将各分量进行合成。当铝含量为39.56mg/kg时，扩展不确定度为2.51mg/kg(k=2)。针对引起测定不确定度的主要贡献者，通过几种改变测量方法的途径，使其中3 个主要分量分别从0. 019 662、0. 002 412、0.002 74下降为0. 010 085、 0. 001 520、0. 001 66，效果显著，达到了降低影响结果准确性因素的目的。     

电感耦合等离子体质谱法测定锡铅焊料中11种杂质元素

锡铅焊料中的杂质元素对焊点的抗氧化性、润湿性、扩展面积有重要影响,因此对其进行测定意义重大。采用硝酸、氢氟酸溶解样品,选择H₂动态反应池模式测定Fe,标准模式测定Al、P、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,同时以Sc校正Al、P、Fe、Cu,以Cs校正Zn、As、Ag、Cd,以Tl校正Sb、Au、Bi,实现了电感耦合等离子体质谱法(ICP-MS)对锡铅焊料中这11种杂质元素含量的测定。在优化的实验条件下,11种杂质元素校准曲线的相关系数均大于0.999,方法的检出限在0.002~0.80μg/g范围内,测定下限在0.007~2.73μg/g范围内。用建立的实验方法测定锡铅焊料样品中Al、P、Fe、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,平行测定11次结果的相对标准偏差(RSD)为0.85%~3.5%,加标回收率为90%~110%。将实验方法应用于锡铅焊料标准物质YT9302中Al、Fe、Cu、Zn、As、Sb、Bi共7种杂质元素的测定,结果与认定值一致。     

Disease Ionomics: Understanding the Role of Ions in Complex Disease

Ionomics is a novel multidisciplinary field that uses advanced techniques to investigate the composition and distribution of all minerals and trace elements in a living organism and their variations under diverse physiological and pathological conditions. It involves both high-throughput elemental profiling technologies and bioinformatic methods, providing opportunities to study the molecular mechanism underlying the metabolism, homeostasis, and cross-talk of these elements. While much effort has been made in exploring the ionomic traits relating to plant physiology and nutrition, the use of ionomics in the research of serious diseases is still in progress. In recent years, a number of ionomic studies have been carried out for a variety of complex diseases, which offer theoretical and practical insights into the etiology, early diagnosis, prognosis, and therapy of them. This review aims to give an overview of recent applications of ionomics in the study of complex diseases and discuss the latest advances and future trends in this area. Overall, disease ionomics may provide substantial information for systematic understanding of the properties of the elements and the dynamic network of elements involved in the onset and development of diseases.     

水提法提取—电感耦合等离子体质谱法测定婴幼儿配方奶粉中的碘

用水提取婴幼儿奶粉中的碘,亚铁氰化钾和乙酸锌盐析法沉淀蛋白,过滤后可以得到澄清处理液。用电感耦合等离子体质谱对提取样液进行测定,130Te作为内标物进行定量分析。该方法简便快捷,检出限为0.10 mg/kg加标回收率为90.8%~109%,相关系数0.999,精密度试验RSD2%。     

环境土壤样品微波消解及钚的ICP-MS测量

钚是环境放射性污染调查和核事故应急监测重点关注的污染核素，土壤样品中钚的定量分析包括样品消解、化学分离和仪器测量等3个步骤。为缩短样品消解时间、提高化学分离效率，对土壤样品微波消解和钚的阴离子交换分离进行了研究，建立了微波消解-阴离子交换分离-电感耦合等离子体质谱（ICP-MS）测量 同位素稀释法定量分析污染土壤样品中²³⁹Pu的流程。以6 mol/L盐酸为浸取试剂，在浸取液体积与土壤质量之比为4∶1~5∶1 mL/g时，5 g土壤样品中²³⁹Pu的加标回收率大于99%。以氢氟酸、硝酸和盐酸的混酸为消解试剂，在氢氟酸浓度为13.2 mol/L时，1 g土壤样品中²³⁹Pu的加标回收率大于94%。用所建流程测得的IAEA-375土壤标准样品中²³⁹Pu的含量与参考值无显著差异，该流程对1 g土壤样品中²³⁹Pu的检出限为84 mBq/kg。     

Quantitative Elemental Analysis of a Single Cell by Using Inductively Coupled Plasma-Mass Spectrometry in Fast Time-Resolved Analysis Mode

The elemental composition of a single yeast, green alga, or red blood cell (RBC) was precisely determined by using inductively coupled plasma-mass spectrometry (ICP-MS) operating in fast time-resolved analysis (TRA) mode. The technique is known as single-cell (SC)-ICP-MS. Phosphorus, sulfur, magnesium, zinc, and iron were detected in the three types of cell. The elemental composition of yeast and green alga obtained by SC-ICP-MS was consistent with results obtained from conventional ICP-MS measurements following acid digestion of the cells. Slight differences were found in the measured values between SC-ICP-MS and the conventional ICP-MS results for RBC. However, the SC-ICP-MS results for S and Fe in RBC were closer to the estimated values for these elements that were calculated from the level of hemoglobin in RBCs. The data suggest that SC-ICP-MS is suitable for the analysis of various cell types, namely, fungus, plant, and animal cells.     

微波消解-ICP-MS法测定舒尼铂原料药中银的残留量

采用微波消解法进行样品前处理，以电感耦合等离子体质谱法(ICP-MS)测定了舒尼铂原料药中的银残留量。结果表明，银质量浓度在0.1~150 μg/L的范围内，与银信号强度和内标铟信号强度的比值呈良好的线性关系，重复性试验的RSD为2.32%，加标回收率为95.89%~104.81%，检出限为0.0109 μg/g，定量限为0.0365 μg/g；3批样品测定结果分别为2.42、1.54和1.96 μg/g。方法可满足舒尼铂原料药中银残留量测定的要求。     

电感耦合等离子体质谱法测定铅锌矿中镓铟锗铊

稀散元素是铅锌矿石中重要的伴生元素,为了综合利用铅锌矿资源,在地质、选矿上经常要考查稀散元素镓、锗、铟、铊的含量。研究了利用电感耦合等离子体质谱法测定铅锌矿中镓、铟、锗、铊4种稀散元素,选取了最佳仪器分析条件,通过在线加入内标校正基体效应和接口效应,检出限分别为0.02μg·g-1、0.01μg·g-1、0.03μg·g-1和0.05μg·g-1,相对标准偏差(RSD)为0.85%~2.84%,回收率在93.3%~102.3%之间,明显优于其他分析方法。该方法样品前处理简便、快捷,测定结果准确,令人满意。     

超级微波消解-ICP-MS法测定塑料中锡元素

通过试验,对超级微波消解条件和电感耦合等离子体质谱仪工作条件进行了优化,建立了超级微波消解-电感耦合等离子体质谱法快速测定塑料中的锡元素含量的方法。本方法的检出限为0.07 mg/kg,RSD为1.9%,多种材料的回收率为91%~107%。结果显示方法有良好的准确度,适用于多种塑料材料中Sn的快速分析。     

电感耦合等离子体质谱法测定小麦粉中铅及其不确定度评定

通过建立数学模型,对电感耦合等离子体质谱法测定小麦粉中的铅的进行不确定度评定。分析并计算了各不确定度分量,计算合成标准不确定度和扩展不确定度。结果表明,方法测量不确定度主要由曲线校正和样品测试重复性引入,而定容体积和称样过程的不确定度可忽略不计。