LC–MS analysis of trimethoxyamphetamine designer drugs (TMA series) from urine samples
A sensitive liquid chromatography–mass spectrometric (LC–MS) method for quantification of an active psychedelic hallucinogenic drugs (trimethoxyamphetamines) in human urine after solid-phase extraction (SPE) with C 18 cartridge was developed and validated. Chromatographic separation was achieved on...
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Veröffentlicht in: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2008-05, Vol.867 (1), p.126-130 |
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container_title | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences |
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creator | Nieddu, Maria Boatto, Gianpiero Pirisi, Maria Antonietta Azara, Emanuela Marchetti, Mauro |
description | A sensitive liquid chromatography–mass spectrometric (LC–MS) method for quantification of an active psychedelic hallucinogenic drugs (trimethoxyamphetamines) in human urine after solid-phase extraction (SPE) with C
18 cartridge was developed and validated. Chromatographic separation was achieved on reversed-phase Phenomenex 3.0
μm Polar Plus column (150
mm
×
2.1
mm) with acetonitrile −0.2% acetic acid as mobile-phase and the step gradient elution resulted in a total run time of about 20
min. The analytes were detected by using an electrospray positive ionization mass spectrometry in selected ion monitoring (SIM) mode. In the evaluated concentration range (10–200
ng/mL) (
R
2
≥
0.998) a good linear relationship was obtained. The lower limits of detection (LLODs) and quantification (LLOQs) ranged from 4.26 to 9.12
ng/mL and from 13.18 to 29.22
ng/mL, respectively. Average recoveries ranged from 68.52 to 97.90% in urine at the concentrations of 25, 50 and 100
ng/mL. Intra- and inter-day relative standard deviations were 3.70–10.77% and 7.63–12.94%, respectively. This LC–MS method proved to be robust and reliable, and suitable for the use as a confirmation method in clinical urine drug testing. |
doi_str_mv | 10.1016/j.jchromb.2008.03.027 |
format | Article |
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18 cartridge was developed and validated. Chromatographic separation was achieved on reversed-phase Phenomenex 3.0
μm Polar Plus column (150
mm
×
2.1
mm) with acetonitrile −0.2% acetic acid as mobile-phase and the step gradient elution resulted in a total run time of about 20
min. The analytes were detected by using an electrospray positive ionization mass spectrometry in selected ion monitoring (SIM) mode. In the evaluated concentration range (10–200
ng/mL) (
R
2
≥
0.998) a good linear relationship was obtained. The lower limits of detection (LLODs) and quantification (LLOQs) ranged from 4.26 to 9.12
ng/mL and from 13.18 to 29.22
ng/mL, respectively. Average recoveries ranged from 68.52 to 97.90% in urine at the concentrations of 25, 50 and 100
ng/mL. Intra- and inter-day relative standard deviations were 3.70–10.77% and 7.63–12.94%, respectively. This LC–MS method proved to be robust and reliable, and suitable for the use as a confirmation method in clinical urine drug testing.</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2008.03.027</identifier><identifier>PMID: 18417429</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Amphetamines - urine ; Analysis ; Analytical, structural and metabolic biochemistry ; Biological and medical sciences ; Chromatography, Liquid - methods ; Designer Drugs ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; Human urine ; Humans ; Liquid chromatography ; Magnetic Resonance Spectroscopy ; Mass spectrometry ; Medical sciences ; Pharmacology. Drug treatments ; Reproducibility of Results ; Sensitivity and Specificity ; Spectrometry, Mass, Electrospray Ionization - methods ; TMA series ; Trimethoxyamphetamines</subject><ispartof>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2008-05, Vol.867 (1), p.126-130</ispartof><rights>2008 Elsevier B.V.</rights><rights>2008 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c488t-1ff251a912abb36f73d318ff420a4b38024f7b5cf88e74a25c9edb29c2b199f83</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S1570023208002006$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=20337892$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/18417429$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Nieddu, Maria</creatorcontrib><creatorcontrib>Boatto, Gianpiero</creatorcontrib><creatorcontrib>Pirisi, Maria Antonietta</creatorcontrib><creatorcontrib>Azara, Emanuela</creatorcontrib><creatorcontrib>Marchetti, Mauro</creatorcontrib><title>LC–MS analysis of trimethoxyamphetamine designer drugs (TMA series) from urine samples</title><title>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences</title><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><description>A sensitive liquid chromatography–mass spectrometric (LC–MS) method for quantification of an active psychedelic hallucinogenic drugs (trimethoxyamphetamines) in human urine after solid-phase extraction (SPE) with C
18 cartridge was developed and validated. Chromatographic separation was achieved on reversed-phase Phenomenex 3.0
μm Polar Plus column (150
mm
×
2.1
mm) with acetonitrile −0.2% acetic acid as mobile-phase and the step gradient elution resulted in a total run time of about 20
min. The analytes were detected by using an electrospray positive ionization mass spectrometry in selected ion monitoring (SIM) mode. In the evaluated concentration range (10–200
ng/mL) (
R
2
≥
0.998) a good linear relationship was obtained. The lower limits of detection (LLODs) and quantification (LLOQs) ranged from 4.26 to 9.12
ng/mL and from 13.18 to 29.22
ng/mL, respectively. Average recoveries ranged from 68.52 to 97.90% in urine at the concentrations of 25, 50 and 100
ng/mL. Intra- and inter-day relative standard deviations were 3.70–10.77% and 7.63–12.94%, respectively. This LC–MS method proved to be robust and reliable, and suitable for the use as a confirmation method in clinical urine drug testing.</description><subject>Amphetamines - urine</subject><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Biological and medical sciences</subject><subject>Chromatography, Liquid - methods</subject><subject>Designer Drugs</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>Human urine</subject><subject>Humans</subject><subject>Liquid chromatography</subject><subject>Magnetic Resonance Spectroscopy</subject><subject>Mass spectrometry</subject><subject>Medical sciences</subject><subject>Pharmacology. Drug treatments</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>TMA series</subject><subject>Trimethoxyamphetamines</subject><issn>1570-0232</issn><issn>1873-376X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2008</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkMtu1DAUhi1ERS_wCCBvQGWR4EsSO6uqGnGTpmJBkbqzHOe441Eug0-CmF3fgTfsk-DRRGXJ6pzF95_LR8hrznLOePVhm2_dJo59kwvGdM5kzoR6Rs64VjKTqrp7nvpSsYwJKU7JOeKWMa6Yki_IKdcFV4Woz8jdevX48OfmO7WD7fYYkI6eTjH0MG3G33vb7zYw2T4MQFvAcD9ApG2c75Fe3t5cU4QYAN9Tny6hczxgmDId4Ety4m2H8GqpF-THp4-3qy_Z-tvnr6vrdeYKraeMey9KbmsubNPIyivZSq69LwSzRSM1E4VXTem81qAKK0pXQ9uI2omG17XX8oK8O87dxfHnDDiZPqCDrrMDjDOaquZFJasDWB5BF0fECN7s0ps27g1n5qDUbM2i1ByUGiZNUppyb5YFc9ND-y-1OEzA2wWw6Gznox1cwCdOMCmVrkXiro4cJB2_AkSDLsDgoA0R3GTaMfznlL9IpZi2</recordid><startdate>20080501</startdate><enddate>20080501</enddate><creator>Nieddu, Maria</creator><creator>Boatto, Gianpiero</creator><creator>Pirisi, Maria Antonietta</creator><creator>Azara, Emanuela</creator><creator>Marchetti, Mauro</creator><general>Elsevier B.V</general><general>Elsevier Science</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>7X8</scope></search><sort><creationdate>20080501</creationdate><title>LC–MS analysis of trimethoxyamphetamine designer drugs (TMA series) from urine samples</title><author>Nieddu, Maria ; Boatto, Gianpiero ; Pirisi, Maria Antonietta ; Azara, Emanuela ; Marchetti, Mauro</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c488t-1ff251a912abb36f73d318ff420a4b38024f7b5cf88e74a25c9edb29c2b199f83</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2008</creationdate><topic>Amphetamines - urine</topic><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Biological and medical sciences</topic><topic>Chromatography, Liquid - methods</topic><topic>Designer Drugs</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>Human urine</topic><topic>Humans</topic><topic>Liquid chromatography</topic><topic>Magnetic Resonance Spectroscopy</topic><topic>Mass spectrometry</topic><topic>Medical sciences</topic><topic>Pharmacology. Drug treatments</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>TMA series</topic><topic>Trimethoxyamphetamines</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Nieddu, Maria</creatorcontrib><creatorcontrib>Boatto, Gianpiero</creatorcontrib><creatorcontrib>Pirisi, Maria Antonietta</creatorcontrib><creatorcontrib>Azara, Emanuela</creatorcontrib><creatorcontrib>Marchetti, Mauro</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>MEDLINE - Academic</collection><jtitle>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Nieddu, Maria</au><au>Boatto, Gianpiero</au><au>Pirisi, Maria Antonietta</au><au>Azara, Emanuela</au><au>Marchetti, Mauro</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>LC–MS analysis of trimethoxyamphetamine designer drugs (TMA series) from urine samples</atitle><jtitle>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences</jtitle><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><date>2008-05-01</date><risdate>2008</risdate><volume>867</volume><issue>1</issue><spage>126</spage><epage>130</epage><pages>126-130</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>A sensitive liquid chromatography–mass spectrometric (LC–MS) method for quantification of an active psychedelic hallucinogenic drugs (trimethoxyamphetamines) in human urine after solid-phase extraction (SPE) with C
18 cartridge was developed and validated. Chromatographic separation was achieved on reversed-phase Phenomenex 3.0
μm Polar Plus column (150
mm
×
2.1
mm) with acetonitrile −0.2% acetic acid as mobile-phase and the step gradient elution resulted in a total run time of about 20
min. The analytes were detected by using an electrospray positive ionization mass spectrometry in selected ion monitoring (SIM) mode. In the evaluated concentration range (10–200
ng/mL) (
R
2
≥
0.998) a good linear relationship was obtained. The lower limits of detection (LLODs) and quantification (LLOQs) ranged from 4.26 to 9.12
ng/mL and from 13.18 to 29.22
ng/mL, respectively. Average recoveries ranged from 68.52 to 97.90% in urine at the concentrations of 25, 50 and 100
ng/mL. Intra- and inter-day relative standard deviations were 3.70–10.77% and 7.63–12.94%, respectively. This LC–MS method proved to be robust and reliable, and suitable for the use as a confirmation method in clinical urine drug testing.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>18417429</pmid><doi>10.1016/j.jchromb.2008.03.027</doi><tpages>5</tpages></addata></record> |
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subjects | Amphetamines - urine Analysis Analytical, structural and metabolic biochemistry Biological and medical sciences Chromatography, Liquid - methods Designer Drugs Fundamental and applied biological sciences. Psychology General pharmacology Human urine Humans Liquid chromatography Magnetic Resonance Spectroscopy Mass spectrometry Medical sciences Pharmacology. Drug treatments Reproducibility of Results Sensitivity and Specificity Spectrometry, Mass, Electrospray Ionization - methods TMA series Trimethoxyamphetamines |
title | LC–MS analysis of trimethoxyamphetamine designer drugs (TMA series) from urine samples |
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