Validation of a high performance liquid chromatographic method for alpha amanitin determination in urine
The objective of the present study was to develop and validate a liquid chromatographic method with electrochemical detection to measure alpha amanitin concentrations in urine after sample pretreatment with double mechanism (reversed phase/cation exchange) solid-phase extraction cartridges. The urin...
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| Veröffentlicht in: | Forensic science international 1998-03, Vol.92 (1), p.59-68 |
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| creator | Defendenti, C Bonacina, E Mauroni, M Gelosa, L |
| description | The objective of the present study was to develop and validate a liquid chromatographic method with electrochemical detection to measure alpha amanitin concentrations in urine after sample pretreatment with double mechanism (reversed phase/cation exchange) solid-phase extraction cartridges. The urine samples (10 ml) were purified and concentrated to 1 ml with elimination of matrix contaminants. The extracts were then separated by isocratic reversed-phase chromatography using a C18 column (4.6 mm×25 cm) with a mobile phase composed of 0.005 M phosphate buffer (pH 7.2) and acetonitrile (90:10). Coulometric detection was performed by applying an oxidation potential of +500 mV to a porous graphite electrode in a low-volume analytical cell. The limit of quantitation was 10 ng/ml with a signal-to-noise ratio=25. The linearity studied on spiked urine was satisfactory (
r=0.9966) from 10 ng/ml to 200 ng/ml. The average extraction recovery of alpha amanitin was 78%, determined using spiked urine samples ranging from 10–300 ng/ml. The intra-assay precision was checked at 10, 50 and 100 ng/ml levels (
n=10) in spiked urine samples, with resulting coefficients of variation of 3.6%, 2% and 1.5%, respectively. |
| doi_str_mv | 10.1016/S0379-0738(98)00006-1 |
| format | Article |
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r=0.9966) from 10 ng/ml to 200 ng/ml. The average extraction recovery of alpha amanitin was 78%, determined using spiked urine samples ranging from 10–300 ng/ml. The intra-assay precision was checked at 10, 50 and 100 ng/ml levels (
n=10) in spiked urine samples, with resulting coefficients of variation of 3.6%, 2% and 1.5%, respectively.</description><identifier>ISSN: 0379-0738</identifier><identifier>EISSN: 1872-6283</identifier><identifier>DOI: 10.1016/S0379-0738(98)00006-1</identifier><identifier>PMID: 9627976</identifier><identifier>CODEN: FSINDR</identifier><language>eng</language><publisher>Kidlington: Elsevier Ireland Ltd</publisher><subject>Accuracy ; Acetonitrile ; Alpha amanitin ; Amanitin ; Amanitins - chemistry ; Amanitins - urine ; Biological and medical sciences ; Cation exchange ; Cation exchanging ; Chromatography ; Chromatography, High Pressure Liquid - methods ; Chromatography, High Pressure Liquid - standards ; Coefficient of variation ; Column chromatography ; Column liquid chromatography ; Contaminants ; Electrochemical analysis ; Electrochemical detection ; Electrochemistry ; Electrodes ; Forensic Medicine ; Humans ; Intoxication ; Mathematical analysis ; Medical sciences ; Mushroom Poisoning - urine ; Mushrooms ; Oxidation ; Plant poisons toxicology ; Poisoning ; Reproducibility of Results ; RNA polymerase ; Signal to noise ratio ; Solid phases ; Toxicology ; Urination ; Urine</subject><ispartof>Forensic science international, 1998-03, Vol.92 (1), p.59-68</ispartof><rights>1998 Elsevier Science Ireland Ltd</rights><rights>1998 INIST-CNRS</rights><rights>1998. Elsevier Science Ireland Ltd</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c514t-28851a78387e7ec7985eb202fde2279e1c4f891f1ac140b203dcd568da284a523</citedby><cites>FETCH-LOGICAL-c514t-28851a78387e7ec7985eb202fde2279e1c4f891f1ac140b203dcd568da284a523</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0379073898000061$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=2203585$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/9627976$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Defendenti, C</creatorcontrib><creatorcontrib>Bonacina, E</creatorcontrib><creatorcontrib>Mauroni, M</creatorcontrib><creatorcontrib>Gelosa, L</creatorcontrib><title>Validation of a high performance liquid chromatographic method for alpha amanitin determination in urine</title><title>Forensic science international</title><addtitle>Forensic Sci Int</addtitle><description>The objective of the present study was to develop and validate a liquid chromatographic method with electrochemical detection to measure alpha amanitin concentrations in urine after sample pretreatment with double mechanism (reversed phase/cation exchange) solid-phase extraction cartridges. The urine samples (10 ml) were purified and concentrated to 1 ml with elimination of matrix contaminants. The extracts were then separated by isocratic reversed-phase chromatography using a C18 column (4.6 mm×25 cm) with a mobile phase composed of 0.005 M phosphate buffer (pH 7.2) and acetonitrile (90:10). Coulometric detection was performed by applying an oxidation potential of +500 mV to a porous graphite electrode in a low-volume analytical cell. The limit of quantitation was 10 ng/ml with a signal-to-noise ratio=25. The linearity studied on spiked urine was satisfactory (
r=0.9966) from 10 ng/ml to 200 ng/ml. The average extraction recovery of alpha amanitin was 78%, determined using spiked urine samples ranging from 10–300 ng/ml. The intra-assay precision was checked at 10, 50 and 100 ng/ml levels (
n=10) in spiked urine samples, with resulting coefficients of variation of 3.6%, 2% and 1.5%, respectively.</description><subject>Accuracy</subject><subject>Acetonitrile</subject><subject>Alpha amanitin</subject><subject>Amanitin</subject><subject>Amanitins - chemistry</subject><subject>Amanitins - urine</subject><subject>Biological and medical sciences</subject><subject>Cation exchange</subject><subject>Cation exchanging</subject><subject>Chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Chromatography, High Pressure Liquid - standards</subject><subject>Coefficient of variation</subject><subject>Column chromatography</subject><subject>Column liquid chromatography</subject><subject>Contaminants</subject><subject>Electrochemical analysis</subject><subject>Electrochemical detection</subject><subject>Electrochemistry</subject><subject>Electrodes</subject><subject>Forensic Medicine</subject><subject>Humans</subject><subject>Intoxication</subject><subject>Mathematical analysis</subject><subject>Medical sciences</subject><subject>Mushroom Poisoning - urine</subject><subject>Mushrooms</subject><subject>Oxidation</subject><subject>Plant poisons toxicology</subject><subject>Poisoning</subject><subject>Reproducibility of Results</subject><subject>RNA polymerase</subject><subject>Signal to noise ratio</subject><subject>Solid phases</subject><subject>Toxicology</subject><subject>Urination</subject><subject>Urine</subject><issn>0379-0738</issn><issn>1872-6283</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1998</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><sourceid>8G5</sourceid><sourceid>BENPR</sourceid><sourceid>GUQSH</sourceid><sourceid>M2O</sourceid><recordid>eNqFkUtr3DAUhUVpSCdpf0JA0FLShVs9Rpa0CiX0BYEs-tiKG-k6VrAtR7IL-fdVMsMsuok2Ap3vXo7OIeSMs4-c8fbTTya1bZiW5tyaD6yetuEvyIYbLZpWGPmSbA7IK3JSyl1llBLtMTm2rdBWtxvS_4EhBlhimmjqKNA-3vZ0xtylPMLkkQ7xfo2B-j6nEZZ0m2Huo6cjLn0KtGIUhrkHChWPS5xowAXzGKfd0vqw5jjha3LUwVDwzf4-Jb-_fvl1-b25uv724_LzVeMV3y6NMEZx0EYajRq9tkbhjWCiCyiqZeR-2xnLOw6eb1lVZPBBtSaAMFtQQp6S97u9c073K5bFjbF4HAaYMK3F8VZaxYWs4Nv_wLu05ql6c8LWpKw0nFVK7SifUykZOzfnOEJ-cJy5xx7cUw_uMWRnjXvqwfE6d7bfvt6MGA5T--Cr_m6vQ_EwdLlmHcsBE_VjyqiKXewwrJH9jZhd8RFrLSFm9IsLKT5j5B-Fr6Rx</recordid><startdate>19980302</startdate><enddate>19980302</enddate><creator>Defendenti, C</creator><creator>Bonacina, E</creator><creator>Mauroni, M</creator><creator>Gelosa, L</creator><general>Elsevier Ireland Ltd</general><general>Elsevier</general><general>Elsevier Limited</general><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>3V.</scope><scope>7QP</scope><scope>7RV</scope><scope>7U7</scope><scope>7X7</scope><scope>7XB</scope><scope>88E</scope><scope>8FE</scope><scope>8FH</scope><scope>8FI</scope><scope>8FJ</scope><scope>8FK</scope><scope>8G5</scope><scope>ABUWG</scope><scope>AFKRA</scope><scope>AZQEC</scope><scope>BBNVY</scope><scope>BENPR</scope><scope>BHPHI</scope><scope>C1K</scope><scope>CCPQU</scope><scope>DWQXO</scope><scope>FYUFA</scope><scope>GHDGH</scope><scope>GNUQQ</scope><scope>GUQSH</scope><scope>HCIFZ</scope><scope>K9.</scope><scope>KB0</scope><scope>LK8</scope><scope>M0S</scope><scope>M1P</scope><scope>M2O</scope><scope>M7P</scope><scope>MBDVC</scope><scope>NAPCQ</scope><scope>PQEST</scope><scope>PQQKQ</scope><scope>PQUKI</scope><scope>Q9U</scope></search><sort><creationdate>19980302</creationdate><title>Validation of a high performance liquid chromatographic method for alpha amanitin determination in urine</title><author>Defendenti, C ; Bonacina, E ; Mauroni, M ; Gelosa, L</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c514t-28851a78387e7ec7985eb202fde2279e1c4f891f1ac140b203dcd568da284a523</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1998</creationdate><topic>Accuracy</topic><topic>Acetonitrile</topic><topic>Alpha amanitin</topic><topic>Amanitin</topic><topic>Amanitins - chemistry</topic><topic>Amanitins - urine</topic><topic>Biological and medical sciences</topic><topic>Cation exchange</topic><topic>Cation exchanging</topic><topic>Chromatography</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Chromatography, High Pressure Liquid - standards</topic><topic>Coefficient of variation</topic><topic>Column chromatography</topic><topic>Column liquid chromatography</topic><topic>Contaminants</topic><topic>Electrochemical analysis</topic><topic>Electrochemical detection</topic><topic>Electrochemistry</topic><topic>Electrodes</topic><topic>Forensic Medicine</topic><topic>Humans</topic><topic>Intoxication</topic><topic>Mathematical analysis</topic><topic>Medical sciences</topic><topic>Mushroom Poisoning - urine</topic><topic>Mushrooms</topic><topic>Oxidation</topic><topic>Plant poisons toxicology</topic><topic>Poisoning</topic><topic>Reproducibility of Results</topic><topic>RNA polymerase</topic><topic>Signal to noise ratio</topic><topic>Solid phases</topic><topic>Toxicology</topic><topic>Urination</topic><topic>Urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Defendenti, C</creatorcontrib><creatorcontrib>Bonacina, E</creatorcontrib><creatorcontrib>Mauroni, M</creatorcontrib><creatorcontrib>Gelosa, L</creatorcontrib><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>ProQuest Central (Corporate)</collection><collection>Calcium & Calcified Tissue Abstracts</collection><collection>ProQuest Nursing & Allied Health Database</collection><collection>Toxicology Abstracts</collection><collection>Health & Medical Collection</collection><collection>ProQuest Central (purchase pre-March 2016)</collection><collection>Medical Database (Alumni Edition)</collection><collection>ProQuest SciTech Collection</collection><collection>ProQuest Natural Science Collection</collection><collection>Hospital Premium Collection</collection><collection>Hospital Premium Collection (Alumni Edition)</collection><collection>ProQuest Central (Alumni) (purchase pre-March 2016)</collection><collection>Research Library (Alumni Edition)</collection><collection>ProQuest Central (Alumni)</collection><collection>ProQuest Central</collection><collection>ProQuest Central Essentials</collection><collection>Biological Science Collection</collection><collection>ProQuest Central</collection><collection>ProQuest Natural Science Collection</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ProQuest One Community College</collection><collection>ProQuest Central</collection><collection>Health Research Premium Collection</collection><collection>Health Research Premium Collection (Alumni)</collection><collection>ProQuest Central Student</collection><collection>Research Library Prep</collection><collection>SciTech Premium Collection</collection><collection>ProQuest Health & Medical Complete (Alumni)</collection><collection>Nursing & Allied Health Database (Alumni Edition)</collection><collection>ProQuest Biological Science Collection</collection><collection>Health & Medical Collection (Alumni Edition)</collection><collection>Medical Database</collection><collection>ProQuest Research Library</collection><collection>Biological Science Database</collection><collection>Research Library (Corporate)</collection><collection>Nursing & Allied Health Premium</collection><collection>ProQuest One Academic Eastern Edition (DO NOT USE)</collection><collection>ProQuest One Academic</collection><collection>ProQuest One Academic UKI Edition</collection><collection>ProQuest Central Basic</collection><jtitle>Forensic science international</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Defendenti, C</au><au>Bonacina, E</au><au>Mauroni, M</au><au>Gelosa, L</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Validation of a high performance liquid chromatographic method for alpha amanitin determination in urine</atitle><jtitle>Forensic science international</jtitle><addtitle>Forensic Sci Int</addtitle><date>1998-03-02</date><risdate>1998</risdate><volume>92</volume><issue>1</issue><spage>59</spage><epage>68</epage><pages>59-68</pages><issn>0379-0738</issn><eissn>1872-6283</eissn><coden>FSINDR</coden><abstract>The objective of the present study was to develop and validate a liquid chromatographic method with electrochemical detection to measure alpha amanitin concentrations in urine after sample pretreatment with double mechanism (reversed phase/cation exchange) solid-phase extraction cartridges. The urine samples (10 ml) were purified and concentrated to 1 ml with elimination of matrix contaminants. The extracts were then separated by isocratic reversed-phase chromatography using a C18 column (4.6 mm×25 cm) with a mobile phase composed of 0.005 M phosphate buffer (pH 7.2) and acetonitrile (90:10). Coulometric detection was performed by applying an oxidation potential of +500 mV to a porous graphite electrode in a low-volume analytical cell. The limit of quantitation was 10 ng/ml with a signal-to-noise ratio=25. The linearity studied on spiked urine was satisfactory (
r=0.9966) from 10 ng/ml to 200 ng/ml. The average extraction recovery of alpha amanitin was 78%, determined using spiked urine samples ranging from 10–300 ng/ml. The intra-assay precision was checked at 10, 50 and 100 ng/ml levels (
n=10) in spiked urine samples, with resulting coefficients of variation of 3.6%, 2% and 1.5%, respectively.</abstract><cop>Kidlington</cop><pub>Elsevier Ireland Ltd</pub><pmid>9627976</pmid><doi>10.1016/S0379-0738(98)00006-1</doi><tpages>10</tpages></addata></record> |
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| identifier | ISSN: 0379-0738 |
| ispartof | Forensic science international, 1998-03, Vol.92 (1), p.59-68 |
| issn | 0379-0738 1872-6283 |
| language | eng |
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| source | MEDLINE; Elsevier ScienceDirect Journals Complete |
| subjects | Accuracy Acetonitrile Alpha amanitin Amanitin Amanitins - chemistry Amanitins - urine Biological and medical sciences Cation exchange Cation exchanging Chromatography Chromatography, High Pressure Liquid - methods Chromatography, High Pressure Liquid - standards Coefficient of variation Column chromatography Column liquid chromatography Contaminants Electrochemical analysis Electrochemical detection Electrochemistry Electrodes Forensic Medicine Humans Intoxication Mathematical analysis Medical sciences Mushroom Poisoning - urine Mushrooms Oxidation Plant poisons toxicology Poisoning Reproducibility of Results RNA polymerase Signal to noise ratio Solid phases Toxicology Urination Urine |
| title | Validation of a high performance liquid chromatographic method for alpha amanitin determination in urine |
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