Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as t...

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Veröffentlicht in:Spectrochimica acta. Part B: Atomic spectroscopy 2015-04, Vol.106, p.13-19
Hauptverfasser: Álvarez Méndez, J., Barciela García, J., García Martín, S., Peña Crecente, R.M., Herrero Latorre, C.
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container_title Spectrochimica acta. Part B: Atomic spectroscopy
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creator Álvarez Méndez, J.
Barciela García, J.
García Martín, S.
Peña Crecente, R.M.
Herrero Latorre, C.
description A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3ngL−1, respectively, and for Pb these limits were 0.13 and 0.43μgL−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n=10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. •Cd and Pb determination based on the combination of DSP, SS and ETAAS•Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes.•Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.•Appropriate detection limits were obtained (9.7ngCdL−1 and 0.13μgPb L−1).•DSP–SS–ETAAS combination allowed a single and high sample throughput procedure.
doi_str_mv 10.1016/j.sab.2015.01.008
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The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3ngL−1, respectively, and for Pb these limits were 0.13 and 0.43μgL−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n=10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. 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Part B: Atomic spectroscopy</title><description>A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3ngL−1, respectively, and for Pb these limits were 0.13 and 0.43μgL−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n=10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. •Cd and Pb determination based on the combination of DSP, SS and ETAAS•Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes.•Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.•Appropriate detection limits were obtained (9.7ngCdL−1 and 0.13μgPb L−1).•DSP–SS–ETAAS combination allowed a single and high sample throughput procedure.</description><subject>Atomic absorption analysis</subject><subject>Cadmium</subject><subject>Carbon nanotube</subject><subject>Dispersive SPE</subject><subject>Electrothermal atomic absorption spectrometry</subject><subject>Extraction</subject><subject>Lead (metal)</subject><subject>Sampling</subject><subject>Slurries</subject><subject>Strategy</subject><subject>Urine</subject><issn>0584-8547</issn><issn>1873-3565</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2015</creationdate><recordtype>article</recordtype><recordid>eNqFkT2O1TAUhSMEEo-BBdC5pEmw49jxiAoNv9JINFBbN_YN-MmxM7Yz8Dr2wH5YDCvBb0I9VJauz_nuz2ma54x2jDL58thlmLqeMtFR1lGqHjQHpkbeciHFw-ZAhRpaJYbxcfMk5yOltBe9ODS_32DBtLgAxcVA4kwM2MVtC4FgiUewxAWyJReQZFhWj5nAXC3Eurxiyu62fkTv7J-fv7y72Zwl-KMkMDsvkGXzxX0H79FWdppqKUCIZZsqajqR7LeUTjvcha8EPZqSYvlWxwJPoMTFGQJTjmm9Y9a2Z8GCJZ2eNo9m8Bmf_Xsvmi_v3n6--tBef3r_8er1dWu45KW1EqUdwCAzcuKXQk4SR2rmYR4HezlI1QuA0Y6TlP08CIvKcsa4tAqNmqnlF82LnbumeLNhLnpx2aD3EDBuWTNF6cBHOYr_S0feK8Yo51XKdqlJMeeEs16TWyCdNKP6HKs-6hqrPseqKdM11up5tXuwrnvrMOlsHAaD1qV6F22ju8f9F_sZsrY</recordid><startdate>20150401</startdate><enddate>20150401</enddate><creator>Álvarez Méndez, J.</creator><creator>Barciela García, J.</creator><creator>García Martín, S.</creator><creator>Peña Crecente, R.M.</creator><creator>Herrero Latorre, C.</creator><general>Elsevier B.V</general><scope>AAYXX</scope><scope>CITATION</scope><scope>7QH</scope><scope>7UA</scope><scope>C1K</scope><scope>F1W</scope><scope>H97</scope><scope>L.G</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><orcidid>https://orcid.org/0000-0002-2138-3675</orcidid></search><sort><creationdate>20150401</creationdate><title>Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry</title><author>Álvarez Méndez, J. ; Barciela García, J. ; García Martín, S. ; Peña Crecente, R.M. ; Herrero Latorre, C.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c363t-d6e6d4ace1c6b3956b6e70cf4f74d946825aa7d7b662f45de8d31136d8ec8f0d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2015</creationdate><topic>Atomic absorption analysis</topic><topic>Cadmium</topic><topic>Carbon nanotube</topic><topic>Dispersive SPE</topic><topic>Electrothermal atomic absorption spectrometry</topic><topic>Extraction</topic><topic>Lead (metal)</topic><topic>Sampling</topic><topic>Slurries</topic><topic>Strategy</topic><topic>Urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Álvarez Méndez, J.</creatorcontrib><creatorcontrib>Barciela García, J.</creatorcontrib><creatorcontrib>García Martín, S.</creatorcontrib><creatorcontrib>Peña Crecente, R.M.</creatorcontrib><creatorcontrib>Herrero Latorre, C.</creatorcontrib><collection>CrossRef</collection><collection>Aqualine</collection><collection>Water Resources Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ASFA: Aquatic Sciences and Fisheries Abstracts</collection><collection>Aquatic Science &amp; Fisheries Abstracts (ASFA) 3: Aquatic Pollution &amp; Environmental Quality</collection><collection>Aquatic Science &amp; Fisheries Abstracts (ASFA) Professional</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Spectrochimica acta. 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The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3ngL−1, respectively, and for Pb these limits were 0.13 and 0.43μgL−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n=10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. •Cd and Pb determination based on the combination of DSP, SS and ETAAS•Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes.•Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.•Appropriate detection limits were obtained (9.7ngCdL−1 and 0.13μgPb L−1).•DSP–SS–ETAAS combination allowed a single and high sample throughput procedure.</abstract><pub>Elsevier B.V</pub><doi>10.1016/j.sab.2015.01.008</doi><tpages>7</tpages><orcidid>https://orcid.org/0000-0002-2138-3675</orcidid></addata></record>
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subjects Atomic absorption analysis
Cadmium
Carbon nanotube
Dispersive SPE
Electrothermal atomic absorption spectrometry
Extraction
Lead (metal)
Sampling
Slurries
Strategy
Urine
title Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry
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