Stanberry Jordan S, Andrews Hunter B, Thompson Cyril V, Ticknor Brian W, Manard Benjamin T
Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37830, United States.
Radioisotope Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37830, United States.
Anal Chem. 2025 Jan 28;97(3):1688-1694. doi: 10.1021/acs.analchem.4c04794. Epub 2025 Jan 10.
A novel employment of single particle-inductively coupled plasma-mass spectrometry (SP-ICP-MS) was developed, where a microextraction (ME) probe is used to sample nanoparticles from a surface and analyze them in a single analytical step. The effects of several parameters on the performance of ME-SP-ICP-MS were investigated, including the flow rate, choice of carrier solution, particle size, and the design of the microextraction probe head itself. The optimized ME-SP-ICP-MS technique was used to compare the extraction efficiency (EE, defined as the ratio of particles measured to particles deposited on the surface) of the commercial probe head to a newly designed SP polyether ether ketone (PEEK) probe head. The SP PEEK probe head was found to have increased EE compared to the commercial probe head (8.5 ± 3% vs 3.9 ± 3%, respectively). Increasing the carrier solution flow rate was found to decrease the total analysis time at the cost of decreasing EE. Extraction efficiencies for ME-SP-ICP-MS were typically 4-10%, which is similar to transport efficiencies (1-10%) for conventional SP-ICP-MS. Lastly, ME-SP-ICP-MS was employed for the analysis of nano- and microparticles. The sizes of gold nanoparticles, 30 ± 3 and 51 ± 1.9 nm (certified sizes), and iron-based microparticles, 1000 ± 50 nm (certified size), were accurately determined to be 32.2 ± 2.5, 50.8 ± 3.4, and 1030 ± 57 nm, respectively, by ME-SP-ICP-MS. This work demonstrates the potential of ME-SP-ICP-MS for the direct analysis of particles on common collection surfaces (GSR tabs, carbon planchettes, etc.) while retaining spatial information on particle distribution across the surface.
开发了一种单颗粒电感耦合等离子体质谱（SP-ICP-MS）的新应用，其中使用微萃取（ME）探针从表面对纳米颗粒进行采样，并在单个分析步骤中对其进行分析。研究了几个参数对ME-SP-ICP-MS性能的影响，包括流速、载液选择、颗粒大小以及微萃取探头本身的设计。使用优化后的ME-SP-ICP-MS技术比较了商业探头与新设计的SP聚醚醚酮（PEEK）探头的萃取效率（EE，定义为测量的颗粒数与沉积在表面的颗粒数之比）。结果发现，与商业探头相比，SP PEEK探头的EE有所提高（分别为8.5±3%和3.9±3%）。发现增加载液流速会以降低EE为代价减少总分析时间。ME-SP-ICP-MS的萃取效率通常为4-10%，这与传统SP-ICP-MS的传输效率（1-10%）相似。最后，ME-SP-ICP-MS用于分析纳米颗粒和微米颗粒。通过ME-SP-ICP-MS准确测定出金纳米颗粒的尺寸（认证尺寸为30±3和51±1.9 nm）以及铁基微米颗粒的尺寸（认证尺寸为1000±50 nm）分别为32.2±2.5、50.8±3.4和1030±57 nm。这项工作证明了ME-SP-ICP-MS在直接分析常见收集表面（GSR标签、碳平板等）上的颗粒同时保留颗粒在表面分布的空间信息方面的潜力。
