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Nanoparticles - a target for speciation analysis


Chemical species are defined by the International Union of Pure and Applied Chemistry (IUPAC) as “specific form of an element defined as to isotopic composition, electronic or oxidation state, and/or complex or molecular structure”. The speciation of elements is mandatory for understanding their mobility in the environment, their uptake by organisms, their biological activities and toxicity. Nanoparticles (NPs) are discrete solid pieces of material with at least one dimension in the size range of 1 to 100 nm. Inorganic NPs can be considered a distinct chemical species of elements themselves, and their analysis can therefore be discussed as part of speciation analysis.  

In this sense the most simple analytical task is the differentiation of the particular species from the dissolved species. However, more specific characterization is needed to understand the bahavior of NPs in different environmental compartments or organisms.

Nanoparticle size: The size of nanoparticles is critically important in various fields and applications due to the profound impact it has on their properties, behaviors, and performance. Here are some key reasons why nanoparticle size is important:

  • Surface Area-to-Volume Ratio: As nanoparticles get smaller, their surface area relative to their volume increases significantly. This high surface area is advantageous for various applications, including catalysis, sensors, and drug delivery, as it provides more active sites for interactions with other substances.
  • Optical Properties: Nanoparticle size can strongly influence their optical properties, such as absorption, scattering, and emission of light. This is crucial in fields like nanophotonics, plasmonics, and the development of nanoscale optical materials.
  • Electromagnetic Properties: In nanoelectronics and nanomaterials, the size of nanoparticles can affect their electrical and magnetic properties, making them suitable for specific electronic or magnetic applications.
  • Catalysis: Smaller nanoparticles often exhibit higher catalytic activity due to their increased surface area, making them valuable in catalytic reactions.
  • Drug Delivery: The size of nanoparticles is critical in drug delivery systems, as it affects their ability to cross biological barriers, target specific cells or tissues, and release drugs in a controlled manner.
  • Toxicity and Biocompatibility: In the field of nanotoxicology and nanomedicine, nanoparticle size can significantly influence their toxicity and biocompatibility. Smaller nanoparticles may have different interactions with biological systems compared to larger ones.
  • Stability and Aggregation: Nanoparticle size can impact their stability in colloidal solutions. Smaller nanoparticles are often more prone to aggregation due to increased Brownian motion, which can affect their performance and applications.
  • Drug Solubility and Bioavailability: In pharmaceuticals, the size of nanoparticles can improve the solubility of poorly water-soluble drugs, increasing their bioavailability.
  • Imaging: Nanoparticle size is crucial in biomedical imaging techniques like magnetic resonance imaging (MRI) and computed tomography (CT) scanning, as it affects the contrast and distribution of imaging agents.
  • Mechanical Properties: In nanomaterials and nanocomposites, nanoparticle size can influence the mechanical properties of the materials, such as strength, stiffness, and toughness.
  • Transport and Diffusion: The size of nanoparticles affects their transport and diffusion properties, which is important in applications like filtration, membrane technologies, and drug transport through biological barriers.
  • Environmental and Ecological Impact: In environmental science, understanding the size distribution of nanoparticles is critical for assessing their transport, behavior, and potential ecological impact in natural systems.

In summary, the size of nanoparticles is a fundamental parameter that influences their performance and behavior in various applications, making it a critical factor to consider when designing, characterizing, and utilizing nanoparticles in science and technology.

Nanoparticle composition:
Nanoparticles may be consistent of a single constituent, or are formed by two or more components. In case of a single component, speciation analyses may involve determining the chemical state or oxidation state of metal nanoparticles. For example, in the case of metal nanoparticles, speciation analysis may aim to distinguish between metallic, oxide, or other forms of the same metal.

Figure: Core-Shell Nanoparticle 
© Creative Commons

Some nanoparticles are designed with a core-shell structure, where different materials are present in the core and the shell. Speciation analysis can be used to determine the composition, structure, and distribution of materials in such nanoparticles.

Engineered nanomaterials are nowadays widely integrated into consumer and industrial products. Besides cosmetic and cleaning products, food is a major source of exposure of consumers to NPs through ingestion. Also nanomaterials released to the environment can be taken up by organisms and re-enter the food web. Even further, NPs can be formed naturally in the environment or in-vivo by the organisms themselves. In order to characterize and quantify NPs in products and in the environment, several analytical techniques have been developed or adapted.

Among these techniques are single-particle ICP-MS and ICP-MS coupled to separation techniques like field flow fractionation (FFF), capillary electrophoresis (CE), hydrodynamic chromatography (HDC) and reversed phase HPLC. Bio-imaging techniques such as laser ablation ICP-MS, nanoscale secondary ion mass spectrometry (nano-SIMS) and X-ray fluorescence support the qualitative analysis of NPs, whereas electron microscopy is typically considered the gold standard when it comes to determination of particle sizes. Electron microscopy provides additional information on particle shape, crystal structure and if
combined with Energy Dispersive X-ray Spectroscopy (EDS), chemical composition can be determined.

Especially challenging is the sample preparation as NPs can agglomerate, aggregate, dissolve or change their crystalline structure or chemical composition. They interact with matrix components and surfaces and might undergo changes.

Apart from size and composition, there are other parameters defining the characteristics of nanoparticles that have to be evaluated by methods beyond speciation analysis, such as nanoparticle coatings, surface functionalization, particle shape or aggregation.

Figure: Lead-Sulfide Nanoparticle, 
passivated with with oleic acid,
oleyl amine and hydroxyl ligands
© Creative Commons

Nanoparticle coating

Many nanoparticles have coatings or surface modifications, such as organic ligands, polymers, or surfactants. Nanoparticle analysis may involve characterizing the nature and composition of these coatings, as they can significantly impact the nanoparticles' behavior and interactions.

Nanoparticle Surface Functionalization
Understanding the nature of functional groups or chemical modifications on the nanoparticle surface is another aspect of nanoparticle analysis, especially for nanoparticles used in various applications like drug delivery or catalysis.

Nanoparticle Aggregates and Clusters

Nanoparticle analysis can help identify the specific forms or arrangements of nanoparticles within aggregates or clusters, which can affect their properties and reactivity.

For a complete understanding of the behavior of NPs, often a combination of several analytical techniques is required.

The following listing gives access to the major topics discussed in the framework of NPs analysis.

Regulations and legislation

Faraat Ali, Kumari Neha, Sana Parveen, Current regulatory landscape of nanomaterials and nanomedicines: A global perspective, J. Drug Deliv. Sci. Technol., 80 (2023) 104118. DOI: 10.1016/j.jddst.2022.104118

Ajay Kumar Mishraa, Rajeswari Dasc, Sanket Sahood, Bisworanjita Biswale, Global regulations and legislations on nanoparticles usage and application in diverse horizons, Compr. Anal. Chem., 99 (2022) 261-290. DOI: 10.1016/bs.coac.2021.12.004

Harald R. Tschiche, Frank S. Bierkandt, Otto Creutzenberg, Valerie Fessard, Roland Franz, Bernd Giese, Ralf Greiner, Karl-Heinz Haas, Andrea Haase, Andrea Hartwig, Kerstin Hund-Rinke, Pauline Iden, Charlotte Kromer, Katrin Loeschner, Diana Mutz, Anastasia Rakow, Kirsten Rasmussen, Hubert Rauscher, Hannes Richter, Janosch Schoon, Otmar Schmid, Claudia Som, Günter E.M. Tovar, Paul Westerhoff, Wendel Wohlleben, Andreas Luch, Peter Laux, Environmental considerations and current status of grouping and regulation of engineered nanomaterials, Environ. Nanotechnol. Monit. Manag., 18 (2022) 100707. DOI: 10.1016/j.enmm.2022.100707

Analytical Chemistry of Nanomaterials

J. Labuda, L. J. Johnston, Z. Mester, Z. Gajdosechova, H. Goenaga-Infante, J. Barek, S. Shtykov, Analytical chemistry of engineered nanomaterials: Part 1. Scope, regulation, legislation, and metrology (IUPAC Technical Report), Pure Appl. Chem.,  95/2 (2023) 133-163. DOI: 10.1515/pac-2021-1001

Ján Labuda, Jiří Barek, Zuzana Gajdosechova, Silvana Jacob, Linda Johnston, Petra Krystek, Zoltan Mester, Josino Moreira, Veronika Svitkova, Kevin J. Wilkinson, Analytical chemistry of engineered nanomaterials: Part 2. analysis in complex samples (IUPAC Technical Report), Pure Appl. Chem., 2023. DOI: 10.1515/pac-2022-0401

Nanomaterials in different matrices

Zuzana Gajdosechova, Katrin Loeschner, Nanoparticles as a younger member of the trace element species family — a food perspective, Anal. Bioanal. Chem., 2023. DOI: 10.1007/s00216-023-04940-z

Sujuan Yu, Zhiqiang Tan, Yujian Lai, Qingcun Li, Jingfu Liu, Nanoparticulate pollutants in the environment: Analytical methods, formation, and transformation, Eco-Environ. Health, 2/2 (2023) 61-73. DOI: 10.1016/j.eehl.2023.04.005

Tawhida Islam, Md. Mizanur Rahaman, Md. Nayem Mia, Iffat Ara, Md. Tariqul Islam, Thoufiqul Alam Riaz, Ana C. J. Araújo, João Marcos Ferreira de Lima Silva, Bruna Caroline Gonçalves Vasconcelos de Lacerda, Edlane Martins de Andrade, Muhammad Ali Khan, Henrique D. M. Coutinho, Zakir Husain, Muhammad Torequl Islam, Therapeutic Perspectives of Metal Nanoformulations, Drugs Drug Candidates, 2/2 (2023) 232-278. DOI: 10.3390/ddc2020014

Abdul Wahab, Asma Munir, Muhammad Hamzah Saleem, Mukhtar Iderawumi AbdulRaheem, Humera Aziz, Manar Fawzi Bani Mfarrej, Gholamreza Abdi, Interactions of Metal‐Based Engineered Nanoparticles with Plants: An Overview of the State of Current Knowledge, Research Progress, and Prospects, J. Plant Growth Regul., 42 (2023) 5396-5416. DOI: 10.1007/s00344-023-10972-7.

Magdalena Borowska, Krzysztof Jankowski, Basic and advanced spectrometric methods for complete nanoparticles characterization in bio/eco systems: current status and future prospects, Anal. Bioanal. Chem., 415 (2023) 4023-4038. DOI: 10.1007/s00216-023-04641-7

Maha M. El-Kady, Iqbal Ansari, Charu Arora, Nidhi Rai, Sanju Soni, Dakeshwar Kumar Verma, Priyanka Singh, Alaa El Din Mahmoud, Nanomaterials: A comprehensive review of applications, toxicity, impact, and fate to environment, J. Mol. Liq-, 370 (2023) 121046. DOI: 10.1016/j.molliq.2022.121046

Shikha Singh, Sheo Mohan Prasad, Gausiya Bashri, Fate and toxicity of nanoparticles in aquatic systems, Acta Geochim., 42 (2023) 63-76. DOI: 10.1007/s11631-022-00572-9

Andreas Gondikas, Julian Alberto Gallego-Urrea, Karin Mattsson, Nanoparticles in the Marine Environment, in: J. Blasco, A. Tovar-Sánchez(eds.), Marine Analytical Chemistry, Springer, 2022, 323-348. DOI: 10.1007/978-3-031-14486-8_7

Dominique Bazin, Nanomaterials in medicine: a concise review of nanomaterials intended to treat pathology, nanomaterials induced by pathology, and pathology provoked by nanomaterials, C.R. Chimie, 25/S3 (2022) 165-188. DOI: 10.5802/crchim.194

Annika Durve Gupta, Sonali Zankar Patil, Potential Environmental Impacts of Nanoparticles Used in Construction Industry, in: J. A. Malik and S. Marathe (eds.), Ecological and Health Effects of Building Materials, Springer, 2022, 159-183. DOI: 10.1007/978-3-030-76073-1_10

Fabienne Séby, Metal and metal oxide nanoparticles in cosmetics and skin care products, in: R. Milacic, J. Scancar, H. Goenaga Infante, J. Vidmar, Analysis and Characterisation of Metal-Based Nanomaterials, Elsevier, 2021, 381-427.  DOI: 10.1016/bs.coac.2021.02.009

Georgios Fytianos, Abbas Rahdar, George Z. Kyzas, Nanomaterials in Cosmetics: Recent Updates, Nanomaterials, 10 (2020) 979. DOI: 10.3390/nano10050979

Abbas Mohajerani, Lucas Burnett, John V. Smith, Halenur Kurmus, John Milas, Arul Arulrajah, Suksun Horpibulsuk, Aeslina Abdul Kadir, Nanoparticles in Construction Materials and Other Applications, and Implications of Nanoparticle Use, Materials, 12 (2019) 3052; DOI: 10.3390/ma12193052

Analytical Techniques for NP Analysis

Qingsheng Bai, Yongguang Yin, Yanwanjing Liu, Haowen Jiang, Mengxin Wu, Weidong Wang, Zhiqiang Tan, Jingfu Liu, Myeong Hee Moon, Baoshan Xing, Flow field-flow fractionation hyphenated with inductively coupled plasma mass spectrometry: a robust technique for characterization of engineered elemental metal nanoparticles in the environment, Appl. Spectros. Rev., 58/2 (2023) 110-131. DOI: 10.1080/05704928.2021.1935272

Ziwei Meng, Lingna Zheng, Hao Fang, Pu Yang, Bing Wang, Liang Li, Meng Wang, Weiyue Feng, Single Particle Inductively Coupled Plasma Time-of-Flight Mass Spectrometry—A Powerful Tool for the Analysis of Nanoparticles in the Environment, Processes, 11/4 (2023) 1237. DOI: 10.3390/pr11041237

Francisco Laborda, Isabel Abad-Alvaro, María S. Jiménez, Eduardo Bolea, Catching particles by atomic spectrometry: Benefits and limitations of single particle - inductively coupled plasma mass spectrometry, Spectrochim. Acta B, 199 (2023) 106570. DOI: 10.1016/j.sab.2022.106570

Jeremie Gouyon, Ariane Boudier, Fatima Barakat, Arnaud Pallotta, Igor Clarot, Taylor dispersion analysis of metallic-based nanoparticles – A short review, Electrophoresis, 43/23-24 (2022) 2377-2391- DOI: 10.1002/elps.202200184

Darya Mozhayeva, Carsten Engelhard, CE Coupled to ICP-MS and Single Particle ICP-MS for Nanoparticle Analysis, in: Christian Neusüß, Kevon Jooß, Capillary Electrophoresis-Mass Spectrometry, Springer, 2022, 243-257. DOI: 10.1007/978-1-0716-2493-7_16

Isabelle A.M. Worms, Vera I. Slaveykova, Asymmetrical Flow Field-Flow Fractionation Coupled to ICP-MS for Characterization of Trace Metal Species in the Environment from Macromolecular to Nano-Assemblage Forms: Current Challenges for Quantification, Chimia 76 (2022) 34–44. DOI: 10.2533/chimia.2022.34

M. Resano, M. Aramendía, E. García-Ruiz, A. Bazo, E. Bolea-Fernandez, F. Vanhaecke, Living in a transient world: ICP-MS reinvented via time-resolved analysis for monitoring single events, Chem. Sci., 13 (2022) 4436. DOI: 10.1039/d1sc05452j

Adam Laycock, Nathaniel J. Clark, Robert Clough, Rachel Smith, Richard D. Handy, Determination of metallic nanoparticles in biological samples by single particle ICP-MS: a systematic review from sample collection to analysis, Environ. Sci.: Nano, 9 (2022) 42. DOI: 10.1039/d1en00680k

Janez Zavašnika, Andreja Šestan, Vasyl Shvalya, Microscopic techniques for the characterisation of metal-based nanoparticles, in: R. Milacic, J. Scancar, H. Goenaga Infante, J. Vidmar, Analysis and Characterisation of Metal-Based Nanomaterials, Elsevier, 2021, 241-284.  DOI: 10.1016/bs.coac.2021.02.006

Marco Roman, Hydrodynamic chromatography for the characterization of inorganic nanoparticles, in: R. Milacic, J. Scancar, H. Goenaga Infante, J. Vidmar, Analysis and Characterisation of Metal-Based Nanomaterials, Elsevier, 2021, 121-171.  DOI: 10.1016/bs.coac.2021.02.005

Heike Traub, Imaging of metal-based nanoparticles in tissue and cell samples by laser ablation inductively coupled plasma mass spectrometry, in: R. Milacic, J. Scancar, H. Goenaga Infante, J. Vidmar, Analysis and Characterisation of Metal-Based Nanomaterials, Elsevier, 2021, 173-240.  DOI: 10.1016/bs.coac.2021.01.006

Maria Montes-Bayón, Jörg Bettmer, The use of high performance liquid chromatography—Inductively coupled plasma-mass spectrometry in the analysis of inorganic nanomaterials, in: R. Milacic, J. Scancar, H. Goenaga Infante, J. Vidmar, Analysis and Characterisation of Metal-Based Nanomaterials, Elsevier, 2021, 285-301.  DOI: 10.1016/bs.coac.2021.02.007

Kenneth Flores, Reagan S. Turley, Carolina Valdes, Yuqing Ye, Jesus Cantu, Jose A. Hernandez-Viezcas, Jason G. Parsons & Jorge L. Gardea-Torresdey, Environmental applications and recent innovations in single particle inductively coupled plasma mass spectrometry (SP-ICP-MS), Appl. Spec. Rev., 56/1 (2021) 1-26. DOI: 10.1080/05704928.2019.1694937

Petra Krystek, Ciprian M. Cirtiu, Hedwig Braakhuis, Margriet Park, Wim H. de Jong, Inductively Coupled Plasma-Mass Spectrometry in Biodistribution Studies of (Engineered) Nanoparticles, in: R.A. Meyers (ed.), Encyclopedia Anal. Chem., wiley, 2019, 1-23.  DOI: 10.1002/9780470027318.a9337.pub2

Stefanos Mourdikoudis, Roger M. Pallares, Nguyen T. K. Thanh, Characterization techniques for nanoparticles: comparison and complementarity upon studying nanoparticle properties, Nanoscale, 10/27 (2018) 12871. DOI: 10.1039/c8nr02278j

Yu-Feng Li, Jiating Zhao, Yuxi Gao, Bai Li, Chunying Chen, Study on the Toxicology of Nanomaterials by Synchrotron Radiation Techniques, in: Chunhai Fan, Zhentang Zhao, Synchrotron Radiation in Materials Science: Light Sources, Techniques, and Applications, Volume 1, Wiley, 2018, 597-631. DOI: 10.1002/9783527697106.ch15

Leena Pitkänen, André M. Striegel, Size-exclusion chromatography of metal nanoparticles and quantum dots, Trends Anal. Chem., 80 (2016) 311-320. DOI: 10.1016/j.trac.2015.06.013

Jan Mast, Eveline Verleysen, Pieter-Jan De Temmerman, Physical Characterization of Nanomaterials in Dispersion by Transmission Electron Microscopy in a Regulatory Framework, in: F.L. Deepak, A. Mayoral, P. Arenal (eds.), Advanced Transmission Electron Microscopy, Springer, 2015, 249-270. DOI: 10.1007/978-3-319-15177-9_8

Bartlomiej Kowalczyk, István Lagzi, Bartosz A. Grzybowski, Nanoseparations: Strategies for size and/or shape-selective purification of nanoparticles, Curr. Opin. Colloid Interface Sci., 16 (2011) 135-148. DOI: 10.1016/j.cocis.2011.01.004

Further chapters on techniques and methodology for speciation analysis:

Chapter 1: Tools for elemental speciation
Chapter 2: ICP-MS - A versatile detection system for speciation analysis
Chapter 3: LC-ICP-MS - The most often used hyphenated system for speciation analysis
Chapter 4: GC-ICP-MS- A very sensitive hyphenated system for speciation analysis
Chapter 5: CE-ICP-MS for speciation analysis
Chapter 6: ESI-MS: The tool for the identification of species
Chapter 7: Speciation Analysis - Striving for Quality
Chapter 8: Atomic Fluorescence Spectrometry as a Detection System for Speciation Analysis
Chapter 9: Gas chromatography for the separation of elemental species
Chapter 10: Plasma source detection techniques for gas chromatography
Chapter 11: Fractionation as a first step towards speciation analysis
Chapter 12: Flow-injection inductively coupled plasma mass spectrometry for speciation analysis
Chapter 13: Gel electrophoresis combined with laser ablation inductively coupled plasma mass spectrometry for speciation analysis
Chapter 14: Non-chromatographic separation techniques for speciation analysis Chapter 19: Chemical speciation modelling
Chapter 21: Chemical vapor generation as a sample introduction technique for speciation analysis
Chapter 23: Isotopic measurements and speciation analysis

last time modified: January 14, 2024

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