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Simple and Fast On-line Speciation of Inorganic Antimony Coupled to ICP-MS


Antimony is a non-essential element both for plants and animals. Its uptake and binding to thiol-containing enzymes is responsible for toxic effects. Its toxicity depends on the species being present, with inorganic species being more toxic than organic species. Even further, the toxicity of inorganic species also depends on its oxidation state, with Sb(III) compounds being ten times more toxic than those of Sb(V). It is obvious that a meaningful risk assessment of antimony occurrence in the environment calls for speciation analysis.

Most methods for antimony speciation analysis are based on either HPLC or electrophoretic separation followed by detection via atomic spectrometric techniques. In case that the speciation analysis can be limited to the differentiation of only two species such as Sb(III) and Sb(V), also non-chromatographic separation methods have been proposed. However, such methods are time-consuming, laborious, and lack of reproducibility if performed by manual operation.

The new study:
A solution to circumvent such manual operation is to use flow techniques with an appropriate manifold, which allow automation of the procedures, reduce the consumption of reagents and improve the reproducibility. A group of researchers from Spain and Brazil have now developed a two-step procedure for the speciation of inorganic antimony. The procedure is fully automated by using a multisyringe flow injection (MSFIA) manifold coupled to ICP-MS.

The developed method is based on a simple two-step procedure with a first selective Sb(III) determination followed by a total inorganic antimony determination after the reduction of Sb(V) to Sb(III). All necessary steps such as sample injection, addition of reducing agent are performed by the MSFIA system. The sensitive detection of Sb(III) is done by hydride generation coupled to ICP-MS. A mini-column packed with an cation exchange resin was used to retain organic antimony species, otherwise interfering with the detection of Sb(III).

Following optimization of the whole procedure using a Box Behnken design, the optimized method was validated with respect to different figures of merit.
Using a sample volume of 2 mL, impressive detection power was obtained with detection limits of 0.016 µg/L for Sb(III) and total inorganic Sb and determination limits of 0.053 µg/l for the same species. The linear working range was 0.053 to 5.0 µg/L. The high reproducibility of the procedure is showing up by the good precision of 1.4% RSD at 0.50 µg/L Sb(III). The two-step procedure is also relatively fast, allowing an analysis frequency of 30 samples per hour.

The accuracy of the method was evaluated by spike recovery tests as proposed by IUPAC for cases where CRMs are not available. Recoveries ranged between 93 and 111% for Sb(III) and 90 to 109% for Sb(V). Finally, the method was applied to the analysis of natural water samples, comprising drinking water, ground water and coastal seawater samples from Majorca Island (Spain).

The authors concluded, that their method demonstrated high selectivity and sensitivity. The automated on-line procedure was also considered to be fast and in accordance with the premise of green chemistry.

The original publication

L.A. Portugal, E. Palacio, V. Cerdŕ, J.H. Santos-Neto, L. Ferrer, S.L.C. Ferreira, Simple and Fast Two-Step Fully Automated Methodology for the Online Speciation of Inorganic Antimony Coupled to ICP-MS. Chemosensors, 10 (2022) 139. DOI: 10.3390/chemosensors10040139

Related studies (newest first):

Z. Zhang, Y. Lu, H. Li, N. Zhang, J. Cao, B. Qiu, Z. Yang, Simultaneous Separation of Sb(III) and Sb(V) by High Performance Liquid Chromatography (HPLC)-Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) with Application to Plants, Soils, and Sediments. Anal. Lett. 2021, 54, 919–934. DOI: 10.1080/00032719.2020.1788049

  X. Ou, C. Wang, M. He, B. Chen, B. Hu, Online simultaneous speciation of ultra-trace inorganic antimony and tellurium in environmental water by polymer monolithic capillary microextraction combined with inductively coupled plasma mass spectrometry. Spectroscopy 2020, 168, 105854. DOI: 10.1016/j.sab.2020.105854

  M. Jabłonska-Czapla, K. Grygoyc, Spatial and temporal variability of metal(loid)s concentration as well as simultaneous determination of five arsenic and antimony species using HPLC-ICP-MS technique in the study of water and bottom sediments of the shallow, lowland, dam reservoir in Poland. Environ. Sci. Pollut. Res. 2020, 27, 12358–12375. DOI: 10.1007/s11356-020-07758-9

  W. Wang, X. Dai, W. Guo, L. Jin, S. Hu, Field-based Speciation of Inorganic Sb Using Ion-exchange Resin Cartridge and ICP-MS Detection. At. Spectrosc. 2020, 41, 74–80. DOI: 10.46770/AS.2020.02.004

  S.L.C. Ferreira, J.P. dos Anjos, C.S.A. Felix, M.M. da Silva Junior, E. Palacio, V. Cerda, Speciation analysis of antimony in environmental samples employing atomic fluorescence spectrometry–Review. Trac-Trends Anal. Chem. 2019, 110, 335–343. DOI: 10.1016/j.trac.2018.11.017

  D. Liu, F. Zhu, W. Ji, H. Liu, Z. Huo, H. Liu, Determination of trace inorganic antimony in PET-bottled soy sauce by ion chromatography-inductively coupled plasma mass spectrometry. Microchem. J. 2019, 151, 104257. DOI: 10.1016/j.microc.2019.104257

L.-Y. Zhao, J.-J. Fei, H.-Z. Lian, L. Mao, X.-B. Cui, Simultaneous speciation analysis of chromium and antimony by novel carboxyl-functionalized hybrid monolithic column solid phase microextraction coupled with ICP-MS. J. Anal. At. Spectrom. 2019, 34, 1693–1700. DOI: 10.1039/c9ja00157c

  M.M.S. Junior, L.A. Portugal, A.M. Serra, L. Ferrer, V. Cerdŕ, S.L. Ferreira, On line automated system for the determination of Sb(V), Sb(III), thrimethyl antimony(v) and total antimony in soil employing multisyringe flow injection analysis coupled to HG-AFS. Talanta 2017, 165, 502–507. DOI: 10.1016/j.talanta.2016.12.022

  L.A. Portugal, L. Ferrer, A.M. Serra, D.G. da Silva, S.L.C. Ferreira, V. Cerdŕ, A non-chromatographic automated system for antimony speciation in natural water exploiting multisyringe flow injection analysis coupled with online hydride generation atomic fluorescence spectrometry. J. Anal. At. Spectrom. 2015, 30, 1133–1141. DOI: 10.1039/c4ja00476k

  S.L.C. Ferreira, W.N. dos Santos, I.F. dos Santos, M.M. Junior, L. Silva, U.A. Barbosa, F.A. de Santana, A.F.D.S. Queiroz, Strategies of sample preparation for speciation analysis of inorganic antimony using hydride generation atomic spectrometry. Microchem. J. 2014, 114, 22–31. DOI: 10.1016/j.microc.2013.11.019

  A.C. Fornieles, A.G. de Torres, E.V. Alonso, M.T.S. Cordero, J.M.C. Pavón, Speciation of antimony(III) and antimony(V) in seawater by flow injection solid phase extraction coupled with online hydride generation inductively coupled plasma mass spectrometry. J. Anal. At. Spectrom. 2011, 26, 1619–1626. DOI: 10.1039/c0ja00273a

  C. Hansen, B. Schmidt, E.H. Larsen, B. Gammelgaard, S. Stürup, H.R. Hansen, Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: New insights into the Sb-chemistry causing poor chromatographic recoveries. Analyst 2011, 136, 996–1002. DOI: 10.1039/c0an00796j

  R. Miravet, J.F. López-Sánchez, R. Rubio, P. Smichowski, G. Polla, Speciation analysis of antimony in extracts of size-classified volcanic ash by HPLC-ICP-MS. Anal. Bioanal. Chem. 2007, 387, 1949–1954. DOI: 10.1007/s00216-006-1077-y

  L. Zhang, Y. Morita, A. Sakuragawa, A. Isozaki, Inorganic speciation of As(III, V), Se(IV, VI) and Sb(III, V) in natural water with GF-AAS using solid phase extraction technology. Talanta 2007, 72, 723–729. DOI: 10.1016/j.talanta.2006.12.001

  S. Amereih, T. Meisel, E. Kahr, W. Wegscheider, Speciation analysis of inorganic antimony in soil using HPLC-ID-ICP-MS. Anal. Bioanal. Chem. 2005, 383, 1052–1059. DOI: 10.1007/s00216-005-0049-y

  N. Semenova, L.O. Leal, R. Forteza, V. Cerdŕ, Antimony determination and speciation by multisyringe flow injection analysis with hydride generation-atomic fluorescence detection. Anal. Chim. Acta 2005, 530, 113–120. DOI: 10.1016/j.aca.2004.08.046

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T.-L. Deng, Y.-W. Chen, N. Belzile, Antimony speciation at ultra trace levels using hydride generation atomic fluorescence spectrometry and 8-hydroxyquinoline as an efficient masking agente. Anal. Chim. Acta 2001, 432, 293–302. DOI: 10.1026/S0003-2670(00)01387-8

M. Krachler, H. Emons, Potential of high-performance liquid chromatography coupled to flow injection hydride generation atomic absorption spectrometry for the speciation of inorganic and organic antimony compounds. J. Anal. At. Spectrom. 2000, 15, 281–285. DOI: 10.1039/A908938j

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last time modified: April 12, 2022


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