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Solid-phase extraction in speciation analysis


SPE for speciation analysis
The SPE process is based on the selective distribution of analytes between the solid extraction material and liquid mobile phase. The analytes are transferred to the solid phase when they possess greater affinity for the solid phase than for the sample matrix. Once retained during the loading step, the analytes are recovered in a second step by elution using a suitable eluent or by thermal desorption into the gas phase. SPE can process large volumes of liquid samples in relatively short time in a reproducible manner.

photo: SPE station
Generally, there are several formats of SPE: SPE cartridges, SPE disks, SPE pipette tips and SPE microcolumns.  Commercial SPE cartridges, disks and pipette tips are widely used, but often operated in an manual off-line mode.

In contrast, the SPE microcolumn can easily be operated on-line coupled to compatible analytical techniques. The separation process can be taylored by selecting the solid phase from a variety of sorbents including reversed phase sorbents, normal phase sorbents, ion exchange sorbents to biological sorbents, carbon nanotubes, graphene, graphene oxide, metal–organic frameworks, mesoporous nanoparticles and functional magnetic nanoparticles, to name only some. Since the interactions between sorbents used for commercial cartridges and target species are not specific, these are most often used for sample clean-up rather than preconcentration of the species.

Speciation studies making use of SPE for species preconcentration and separation are often based on the development of sorbents designed to interact with a given group of species. Strategies to obtain high selectivity of sorbents are based on the use of ion/molecule imprinted materials, biological substrates or nanoparticles. Using nanoparticles as sorbents offers the possibility of surface functionalization for improved analyte selectivity.  

Solid phase microextraction
Miniaturization of SPE has been realized with the development of solid-phase micro-extraction (SPME) in the early 1990s. Beyond miniaturization, SPME integrates sampling, sample preparation, and preconcentration into a single step prior to instrumental analysis with special designed interfaces for  sample introduction. Compared to conventional SPE, SPME features many advantages such as simplicity, rapidity, convenience, and low sample/reagent consumption. Common formats of SPME include fiber SPME, in-tube SPME (also termed as CME), and Stir bar sorptive extraction (SBSE).

SPE/SPME has been widely used in elemental speciation of biological, environmental and food samples because of their excellent matrix tolerance and high EF obtainable during short collection time. SPE is more suited for the analysis of large volume biological samples, while SPME, CME and SBSE are used with smaller volumes, less than 1 mL.

Related Reviews (newest first)

Ivanka Dakova, Tanya Yordanova, Irina Karadjova, Polymeric Materials in Speciation Analysis on Solid-Phase Extraction, Molecules 29/1 (2024) #187. DOI: 10.3390/molecules29010187

I. Morales-Benítez, P. Montoro-Leal, J.C. García-Mesa, J. Verdeja-Galán, E.I. Vereda Alonso, Magnetic graphene oxide as a valuable material for the speciation of trace elements, Trends Anal. Chem., 157 (2022) 116777. DOI: 10.1016/j.trac.2022.116777

Hai-yan Yang, Rui Jian, Jing Liao, Jie Cui, Ping Fang, Zhi-rong Zou, Ke Huang, Recent development of non-chromatographic atomic specztometry for speciation analysis of mercury, Appl. Spectrosc. Rev., 57/6 (2022) 441-460. DOI: 10.1080/05704928.2021.1893183

A.I.C. Ricardo, F. Abujaber, F.J.G. Bernardo, R.C.R. Martín-Doimeadios, A. Rıos, Magnetic solid phase extraction as a valuable tool for elemental speciation analysis, Trends Environ.  Anal. Chem., 27 (2020) e00097. DOI: 10.1016/j.teac.2020.e00097

Krystyna Pyrzynska, Nanomaterials in speciation analysis of metals and metalloids, Talanta, 212 (2020) 120784. DOI: 10.1016/j.talanta.2020.120784

K.K. Jinadasa, E. Pena-Vazquez, P. Bermejo-Barrera, A. Moreda-Pineiro, New adsorbents based on imprinted polymers and composite nanomaterials for arsenic and mercury screening/speciation: A review, Microchem. J., 156 (2020) 104886. DOI: 10.1016/j.microc.2020.104886

Irina Karadjova, Tanya Yordanova, Ivanka Dakova, Penka Vaseleva, Smart Materials in Speciation Analysis, in: M. de la Guardia, F.A. Esteve-Turrillas (eds.), Handbook of Smart Materials in Analytical Chemistry, John Wiley & Sons, Hoboken (2019) 757-793. DOI: 10.1002/9781119422587.ch24

C. Herrero-Latorre, J. Barciela-Garcia, S. Garcia-Martin, R.M. Pena-Crecente, Graphene and carbon nanotubes as solid phase extraction sorbents for the speciation of chromium: A review, Anal. Chim. Acta, 1002 (2018) 1-17. DOI: 10.1016/j.aca.2017.11.042

Ting Yang, Xiao-Yan Wang, Li-Yun Wang, Ming-Li Chen, Jian-Hua Wang, Biological cells in the speciation of heavy metals, Anal. Methods, 8/47 (2016) 8251-8261. DOI: 10.1039/c6ay02324j

Laura Trzonkowska, Barbara Leœniewska, Beata Godlewska-Zylkiewicz, Recent Advances in On-Line Methods Based on Extraction for Speciation Analysis of Chromium in Environmental Matrices, Crit. Rev. Anal. Chem., 46/4 (2016) 305-322. DOI: 10.1080/10408347.2015.1058698

Leticia B. Escudero, Mariángeles Ávila Maniero, Elizabeth Agostini, Patricia N. Smichowski, Biological substrates: Green alternatives in trace elemental preconcentration and speciation analysis, Trends Anal. Chem.  80 (2016) 531–546. DOI: 10.1016/j.trac.2016.04.002

C. Bendicho, C. Bendicho-Lavilla, I. Lavilla, Nanoparticle-assisted chemical speciation of trace elements, Trends Anal. Chem., 77 (2016) 109–121. DOI: 10.1016/j.trac.2015.12.015

Chuan-Ting Liu, An-Na Tang, Applications of Nanoparticles in Elemental Speciation, Anal. Lett., 48/7 (2015)1031-1043. DOI: 10.1080/00032719.2014.976868

D. Das, U. Gupta, A.K. Das, Recent developments in solid phase extraction in elemental speciation of environmenmtal samples with special reference to aqueous solutions, Trends Anal. Chem., 38 (2012) 163-171. DOI: 10.1016/j.trac.2011.01.020

Krystyna Pyrzynska, Carbon nanostructures for separation, preconcentration and speciation of metal ions, Trends Anal. Chem., 29/7 (2010) 718-727. DOI: 10.1016/j.trac.2010.03.013

Ming-Li Chen, Lin-Yu Ma, Xu-Wei Chen, New procedures for arsenic speciation: A review, Talanta, 125 (2014) 78–86. DOI: 10.1016/j.talanta.2014.02.037  

C. Herrero Latorre, J. Barciela Garcia, S. Garcia Martin, R.M. Pena Crecente, Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: A review, Anal. Chim. Acta, 804 (2013) 37– 49. DOI: 10.1016/j.aca.2013.09.054  

Debasis Das, Utpal Gupta, Arabinda K. Das, Recent developments in solid phase extraction in elemental speciation of environmental samples with special reference to aqueous solutions, Trends Anal. Chem., 38 (2012) 163-171. DOI: 10.1016/j.trac.2011.01.020

Krystyna Pyrzynska, Redox speciation of chromium using sorption-based systems, Trends Anal. Chem., 32 (2012) 100-112. DOI: 10.1016/j.trac.2011.09.004

Bin Hu., Fei Zheng, Man He, Nan Zhang, Capillary microextraction (CME) and its application to trace elements analysis and their speciation, Anal.  Chim. Acta, 650 (2009) 23–32. DOI: 10.1016/j.aca.2009.04.002

Sergi Diez, Josep M. Bayona, Determination of Hg and organomercury species following SPME: A review, Talanta, 77 (2008) 21–27. DOI: 10.1016/j.talanta.2008.06.027

Varinder Kaur, Ashok Kumar Malik, Neelam Verma, Applications of solid phase microextraction for the determination of metallic and organometallic species, J. Sep. Sci., 29 (2006) 333 – 345. DOI: 10.1002/jssc.200500319

Ashok Kumar Malik, Varinder Kaur, Neelam Verma, A review on solid phase micro-extraction—High performance liquid chromatography as a novel tool for the analysis of toxic metal ions, Talanta, 68 (2006) 842–849. DOI: 10.1016/j.talanta.2005.06.005

Zoltan Mester, Ralph Sturgeon, Trace element speciation using solid phase microextraction, Spectrochim. Acta B,  60 (2005) 1243 – 1269. DOI: 10.1016/j.sab.2005.06.013

 Related EVISA Resources: Brief summaries

About Speciation

   Speciation as a discipline in Analytical Chemistry – Definitions   
   Why should elemental speciation be done ?
   Why is elemental speciation analysis not done routinely ?
   Speciation analysis as a tool to enhance the quality of life
   Speciation and Toxicity

Research fields related to elemental speciation

   Chemical speciation analysis for the life sciences
   Chemical speciation analysis for nutrition and food science
   Trace element speciation analysis for environmental sciences
   Speciation analysis for the study of metallodrugs and their biomolecular interactions

Speciation Analysis - Striving for Quality

   Problems to be solved in the field of speciation analysis
   Error sources in speciation analysis - Overview
   Sample preservation for speciation analysis - General recommendations
   Species transformation during speciation analysis
   Certified Reference Materials for Chemical Speciation Analysis
   Standard methods for elemental speciation analysis

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 analysislast time modified: January 28, 2024


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