Simultaneous determination of gentisic, salicyluric and salicylic acid in human plasma using solid-phase extraction, liquid chromatography and electrospray ionization mass spectrometry.
Identifieur interne : 001D82 ( Main/Corpus ); précédent : 001D81; suivant : 001D83Simultaneous determination of gentisic, salicyluric and salicylic acid in human plasma using solid-phase extraction, liquid chromatography and electrospray ionization mass spectrometry.
Auteurs : R. Pirker ; C W Huck ; M. Popp ; G K BonnSource :
- Journal of chromatography. B, Analytical technologies in the biomedical and life sciences [ 1570-0232 ] ; 2004.
English descriptors
- KwdEn :
- MESH :
- chemical , blood : Gentisates, Hippurates, Salicylic Acid.
- methods : Chromatography, High Pressure Liquid, Spectrometry, Mass, Electrospray Ionization.
- Calibration, Humans, Reproducibility of Results.
Abstract
A method is developed for the simultaneous extraction of gentisic (GA), salicyluric (SUA) and salicylic acid (SA) in human plasma from Willow Bark extract, by solid phase extraction (SPE) using Waters Oasis HLB (divinylbenzene-n-vinylpyrrolidone copolymer) cartridges. Also, a method is optimized comprising of reversed-phase (RP) high-performance liquid chromatography (HPLC) in connection with electrospray ionization mass spectrometry (ESI-MS), fluorescence detection (FLD) and photo diode array detection (DAD) to identify and quantify GA, SUA and SA in the SPE effluents. An improved sensitivity regarding the lower detection limit (LOD) of < 7 ng/ml, the limit of quantitation (LOQ) of 20 ng/ml and short analysis times of < 15 min is required. The validated SPE method shows linearity in the range of 9.0-58.2 ng/ml for GA, 9.4-191.5 ng/ml for SUA and 12.8-1101.6 ng/ml for SA. The correlation coefficient values are > 0.9994 and 0.99 for fluorescence detection (FLD) and electrospray ionization mass spectrometry (ESI-MS), respectively. The recoveries are from 91.3-102.1% for gentisic acid (GA), 86.8-100.5% for salicyluric acid (SUA) and 75.8-81.4% for salicylic acid (SA) depending on the starting concentrations. RP-LC-ESI-MS/MS studies using collision induced dissociation (CID) confirm that the investigated analytes are not artifacts and facilitate further specific identification in addition to the determination of the parent ion mass even in the presence of co-eluting peaks. The established method is also used to analyze gentisic (GA), salicyluric (SUA) and salicylic acid (SA), not only after intake of Willow Bark capsules (Assalix, BNO 1455) but also as naturally occurring constituents in human plasma after the intake of salicylic acid containing foods.
DOI: 10.1016/j.jchromb.2004.06.031
PubMed: 15315774
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pubmed:15315774Le document en format XML
<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Simultaneous determination of gentisic, salicyluric and salicylic acid in human plasma using solid-phase extraction, liquid chromatography and electrospray ionization mass spectrometry.</title><author><name sortKey="Pirker, R" sort="Pirker, R" uniqKey="Pirker R" first="R" last="Pirker">R. Pirker</name><affiliation><nlm:affiliation>Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 52a, 6020 Innsbruck, Austria.</nlm:affiliation></affiliation></author><author><name sortKey="Huck, C W" sort="Huck, C W" uniqKey="Huck C" first="C W" last="Huck">C W Huck</name></author><author><name sortKey="Popp, M" sort="Popp, M" uniqKey="Popp M" first="M" last="Popp">M. Popp</name></author><author><name sortKey="Bonn, G K" sort="Bonn, G K" uniqKey="Bonn G" first="G K" last="Bonn">G K Bonn</name></author></titleStmt><publicationStmt><idno type="wicri:source">PubMed</idno><date when="2004">2004</date><idno type="RBID">pubmed:15315774</idno><idno type="pmid">15315774</idno><idno type="doi">10.1016/j.jchromb.2004.06.031</idno><idno type="wicri:Area/Main/Corpus">001D82</idno><idno type="wicri:explorRef" wicri:stream="Main" wicri:step="Corpus" wicri:corpus="PubMed">001D82</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en">Simultaneous determination of gentisic, salicyluric and salicylic acid in human plasma using solid-phase extraction, liquid chromatography and electrospray ionization mass spectrometry.</title><author><name sortKey="Pirker, R" sort="Pirker, R" uniqKey="Pirker R" first="R" last="Pirker">R. Pirker</name><affiliation><nlm:affiliation>Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 52a, 6020 Innsbruck, Austria.</nlm:affiliation></affiliation></author><author><name sortKey="Huck, C W" sort="Huck, C W" uniqKey="Huck C" first="C W" last="Huck">C W Huck</name></author><author><name sortKey="Popp, M" sort="Popp, M" uniqKey="Popp M" first="M" last="Popp">M. Popp</name></author><author><name sortKey="Bonn, G K" sort="Bonn, G K" uniqKey="Bonn G" first="G K" last="Bonn">G K Bonn</name></author></analytic><series><title level="j">Journal of chromatography. B, Analytical technologies in the biomedical and life sciences</title><idno type="ISSN">1570-0232</idno><imprint><date when="2004" type="published">2004</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Calibration (MeSH)</term><term>Chromatography, High Pressure Liquid (methods)</term><term>Gentisates (blood)</term><term>Hippurates (blood)</term><term>Humans (MeSH)</term><term>Reproducibility of Results (MeSH)</term><term>Salicylic Acid (blood)</term><term>Spectrometry, Mass, Electrospray Ionization (methods)</term></keywords><keywords scheme="MESH" type="chemical" qualifier="blood" xml:lang="en"><term>Gentisates</term><term>Hippurates</term><term>Salicylic Acid</term></keywords><keywords scheme="MESH" qualifier="methods" xml:lang="en"><term>Chromatography, High Pressure Liquid</term><term>Spectrometry, Mass, Electrospray Ionization</term></keywords><keywords scheme="MESH" xml:lang="en"><term>Calibration</term><term>Humans</term><term>Reproducibility of Results</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">A method is developed for the simultaneous extraction of gentisic (GA), salicyluric (SUA) and salicylic acid (SA) in human plasma from Willow Bark extract, by solid phase extraction (SPE) using Waters Oasis HLB (divinylbenzene-n-vinylpyrrolidone copolymer) cartridges. Also, a method is optimized comprising of reversed-phase (RP) high-performance liquid chromatography (HPLC) in connection with electrospray ionization mass spectrometry (ESI-MS), fluorescence detection (FLD) and photo diode array detection (DAD) to identify and quantify GA, SUA and SA in the SPE effluents. An improved sensitivity regarding the lower detection limit (LOD) of < 7 ng/ml, the limit of quantitation (LOQ) of 20 ng/ml and short analysis times of < 15 min is required. The validated SPE method shows linearity in the range of 9.0-58.2 ng/ml for GA, 9.4-191.5 ng/ml for SUA and 12.8-1101.6 ng/ml for SA. The correlation coefficient values are > 0.9994 and 0.99 for fluorescence detection (FLD) and electrospray ionization mass spectrometry (ESI-MS), respectively. The recoveries are from 91.3-102.1% for gentisic acid (GA), 86.8-100.5% for salicyluric acid (SUA) and 75.8-81.4% for salicylic acid (SA) depending on the starting concentrations. RP-LC-ESI-MS/MS studies using collision induced dissociation (CID) confirm that the investigated analytes are not artifacts and facilitate further specific identification in addition to the determination of the parent ion mass even in the presence of co-eluting peaks. The established method is also used to analyze gentisic (GA), salicyluric (SUA) and salicylic acid (SA), not only after intake of Willow Bark capsules (Assalix, BNO 1455) but also as naturally occurring constituents in human plasma after the intake of salicylic acid containing foods.</div></front></TEI><pubmed><MedlineCitation Status="MEDLINE" Owner="NLM"><PMID Version="1">15315774</PMID><DateCompleted><Year>2005</Year><Month>03</Month><Day>24</Day></DateCompleted><DateRevised><Year>2013</Year><Month>11</Month><Day>21</Day></DateRevised><Article PubModel="Print"><Journal><ISSN IssnType="Print">1570-0232</ISSN><JournalIssue CitedMedium="Print"><Volume>809</Volume><Issue>2</Issue><PubDate><Year>2004</Year><Month>Oct</Month><Day>05</Day></PubDate></JournalIssue><Title>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences</Title><ISOAbbreviation>J Chromatogr B Analyt Technol Biomed Life Sci</ISOAbbreviation></Journal><ArticleTitle>Simultaneous determination of gentisic, salicyluric and salicylic acid in human plasma using solid-phase extraction, liquid chromatography and electrospray ionization mass spectrometry.</ArticleTitle><Pagination><MedlinePgn>257-64</MedlinePgn></Pagination><Abstract><AbstractText>A method is developed for the simultaneous extraction of gentisic (GA), salicyluric (SUA) and salicylic acid (SA) in human plasma from Willow Bark extract, by solid phase extraction (SPE) using Waters Oasis HLB (divinylbenzene-n-vinylpyrrolidone copolymer) cartridges. Also, a method is optimized comprising of reversed-phase (RP) high-performance liquid chromatography (HPLC) in connection with electrospray ionization mass spectrometry (ESI-MS), fluorescence detection (FLD) and photo diode array detection (DAD) to identify and quantify GA, SUA and SA in the SPE effluents. An improved sensitivity regarding the lower detection limit (LOD) of < 7 ng/ml, the limit of quantitation (LOQ) of 20 ng/ml and short analysis times of < 15 min is required. The validated SPE method shows linearity in the range of 9.0-58.2 ng/ml for GA, 9.4-191.5 ng/ml for SUA and 12.8-1101.6 ng/ml for SA. The correlation coefficient values are > 0.9994 and 0.99 for fluorescence detection (FLD) and electrospray ionization mass spectrometry (ESI-MS), respectively. The recoveries are from 91.3-102.1% for gentisic acid (GA), 86.8-100.5% for salicyluric acid (SUA) and 75.8-81.4% for salicylic acid (SA) depending on the starting concentrations. RP-LC-ESI-MS/MS studies using collision induced dissociation (CID) confirm that the investigated analytes are not artifacts and facilitate further specific identification in addition to the determination of the parent ion mass even in the presence of co-eluting peaks. The established method is also used to analyze gentisic (GA), salicyluric (SUA) and salicylic acid (SA), not only after intake of Willow Bark capsules (Assalix, BNO 1455) but also as naturally occurring constituents in human plasma after the intake of salicylic acid containing foods.</AbstractText><CopyrightInformation>Copyright 2004 Elsevier B.V.</CopyrightInformation></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>Pirker</LastName><ForeName>R</ForeName><Initials>R</Initials><AffiliationInfo><Affiliation>Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 52a, 6020 Innsbruck, Austria.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Huck</LastName><ForeName>C W</ForeName><Initials>CW</Initials></Author><Author ValidYN="Y"><LastName>Popp</LastName><ForeName>M</ForeName><Initials>M</Initials></Author><Author ValidYN="Y"><LastName>Bonn</LastName><ForeName>G K</ForeName><Initials>GK</Initials></Author></AuthorList><Language>eng</Language><PublicationTypeList><PublicationType UI="D016428">Journal Article</PublicationType></PublicationTypeList></Article><MedlineJournalInfo><Country>Netherlands</Country><MedlineTA>J Chromatogr B Analyt Technol Biomed Life Sci</MedlineTA><NlmUniqueID>101139554</NlmUniqueID><ISSNLinking>1570-0232</ISSNLinking></MedlineJournalInfo><ChemicalList><Chemical><RegistryNumber>0</RegistryNumber><NameOfSubstance UI="D005841">Gentisates</NameOfSubstance></Chemical><Chemical><RegistryNumber>0</RegistryNumber><NameOfSubstance UI="D006626">Hippurates</NameOfSubstance></Chemical><Chemical><RegistryNumber>487-54-7</RegistryNumber><NameOfSubstance UI="C000693">salicylurate</NameOfSubstance></Chemical><Chemical><RegistryNumber>O414PZ4LPZ</RegistryNumber><NameOfSubstance UI="D020156">Salicylic Acid</NameOfSubstance></Chemical><Chemical><RegistryNumber>VP36V95O3T</RegistryNumber><NameOfSubstance UI="C010925">2,5-dihydroxybenzoic acid</NameOfSubstance></Chemical></ChemicalList><CitationSubset>IM</CitationSubset><MeshHeadingList><MeshHeading><DescriptorName UI="D002138" MajorTopicYN="N">Calibration</DescriptorName></MeshHeading><MeshHeading><DescriptorName UI="D002851" MajorTopicYN="N">Chromatography, High Pressure Liquid</DescriptorName><QualifierName UI="Q000379" MajorTopicYN="Y">methods</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D005841" MajorTopicYN="N">Gentisates</DescriptorName><QualifierName UI="Q000097" MajorTopicYN="Y">blood</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D006626" MajorTopicYN="N">Hippurates</DescriptorName><QualifierName UI="Q000097" MajorTopicYN="Y">blood</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D006801" MajorTopicYN="N">Humans</DescriptorName></MeshHeading><MeshHeading><DescriptorName UI="D015203" MajorTopicYN="N">Reproducibility of Results</DescriptorName></MeshHeading><MeshHeading><DescriptorName UI="D020156" MajorTopicYN="N">Salicylic Acid</DescriptorName><QualifierName UI="Q000097" MajorTopicYN="Y">blood</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D021241" MajorTopicYN="N">Spectrometry, Mass, Electrospray Ionization</DescriptorName><QualifierName UI="Q000379" MajorTopicYN="Y">methods</QualifierName></MeshHeading></MeshHeadingList></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="received"><Year>2003</Year><Month>12</Month><Day>01</Day></PubMedPubDate><PubMedPubDate PubStatus="revised"><Year>2004</Year><Month>06</Month><Day>16</Day></PubMedPubDate><PubMedPubDate PubStatus="accepted"><Year>2004</Year><Month>06</Month><Day>17</Day></PubMedPubDate><PubMedPubDate PubStatus="pubmed"><Year>2004</Year><Month>8</Month><Day>19</Day><Hour>5</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="medline"><Year>2005</Year><Month>3</Month><Day>25</Day><Hour>9</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="entrez"><Year>2004</Year><Month>8</Month><Day>19</Day><Hour>5</Hour><Minute>0</Minute></PubMedPubDate></History><PublicationStatus>ppublish</PublicationStatus><ArticleIdList><ArticleId IdType="pubmed">15315774</ArticleId><ArticleId IdType="doi">10.1016/j.jchromb.2004.06.031</ArticleId><ArticleId IdType="pii">S1570-0232(04)00511-2</ArticleId></ArticleIdList></PubmedData></pubmed></record>Pour manipuler ce document sous Unix (Dilib)
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