Franze Bastian, Engelhard Carsten
University of Münster , Institute of Inorganic and Analytical Chemistry, Corrensstrasse 28/30, 48149 Münster, Germany.
Anal Chem. 2014 Jun 17;86(12):5713-20. doi: 10.1021/ac403998e. Epub 2014 Jun 5.
In this study, a method for separation, size characterization, and speciation of gold and silver nanoparticles was developed through the use of micellar electrokinetic chromatography (MEKC) coupled to inductively coupled plasma-mass spectrometry (ICP-MS) for the first time. Figures of merit in this proof-of-principle study include peak area precision of 4-6%, stable migration times (1.4% with internal standard), and capillary recoveries on the order of 72-100% depending on species and nanoparticle size, respectively. Detection limits are currently in the sub-microgram per liter range. For example, a total of 1500 50-nm-sized gold nanoparticles were successfully detected. After careful optimization, MEKC-ICP-MS was used to separate engineered nanoparticles (ENPs) of different composition. Speciation analysis of ENPs and free metal ions in solution was feasible using a complexing agent (penicillamine). Gold speciation analysis of a dietary supplement, which contained approximately 6-nm-sized gold nanoparticles, was demonstrated.
在本研究中，首次开发了一种通过胶束电动色谱（MEKC）与电感耦合等离子体质谱（ICP-MS）联用的方法，用于金和银纳米颗粒的分离、尺寸表征及形态分析。在这项原理验证研究中的性能指标包括：峰面积精密度为4-6%，迁移时间稳定（使用内标时为1.4%），毛细管回收率根据物种和纳米颗粒大小分别在72-100%左右。目前的检测限在每升亚微克范围内。例如，成功检测到了总共1500个50纳米大小的金纳米颗粒。经过仔细优化后，MEKC-ICP-MS被用于分离不同组成的工程纳米颗粒（ENP）。使用络合剂（青霉胺）对溶液中的ENP和游离金属离子进行形态分析是可行的。对一种含有约6纳米大小金纳米颗粒的膳食补充剂进行了金形态分析。
