Rapid and sensitive screening and selective quantification of antibiotics in human urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

A rapid and sensitive method for the screening and selective quantification of antibiotics in urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was developed. This method allowed the injection of 200 μL urine extract. The 200-μL...

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Veröffentlicht in:Analytical and bioanalytical chemistry 2014-12, Vol.406 (30), p.8049-8058
Hauptverfasser: Wang, He-xing, Wang, Bin, Zhou, Ying, Jiang, Qing-wu
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Wang, Bin
Zhou, Ying
Jiang, Qing-wu
description A rapid and sensitive method for the screening and selective quantification of antibiotics in urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was developed. This method allowed the injection of 200 μL urine extract. The 200-μL injection volume used in this method increased the absolute sensitivity for target antibiotics in solvent by an average 13.3 times, with a range from 8.4 to 28.5 times, compared with the 10-μL conventional injection volume. A 96-well solid phase extraction procedure was established to eliminate the contamination on the chromatographic column resulting from the large-volume injection and increase the throughput of sample preparation. Fourteen target antibiotics from six common categories (β-lactams, quinolones, tetracyclines, macrolides, sulfonamides, and chloramphenicols) were selected as model compounds, and a database containing an additional 74 antibiotics was compiled for posttarget screening. The limit of detection of the target antibiotics, defined as a signal-to-noise ratio of 3, ranged from 0.04 to 1.99 ng/mL. The mean interday recoveries ranged between 79.6 and 121.3 %, with a relative standard deviation from 2.9 to 18.3 % at three spiking levels of 20 ng/mL, 50 ng/mL, and 100 ng/mL. This method was successfully applied in 60 real urine samples from schoolchildren aged 8–11 years, and four target antibiotics (azithromycin, sulfadiazine, trimethoprim, and oxytetracycline) and two posttarget antibiotics (sulfadimidine and cefaclor) were found in the urine samples. This method can be used as a large-scale biomonitoring tool for exposure of the human population to antibiotics. Graphical abstract The analysis procedure of urinary antibiotics by two-dimensional UPLC-Q/TOF MS
doi_str_mv 10.1007/s00216-014-8197-6
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This method allowed the injection of 200 μL urine extract. The 200-μL injection volume used in this method increased the absolute sensitivity for target antibiotics in solvent by an average 13.3 times, with a range from 8.4 to 28.5 times, compared with the 10-μL conventional injection volume. A 96-well solid phase extraction procedure was established to eliminate the contamination on the chromatographic column resulting from the large-volume injection and increase the throughput of sample preparation. Fourteen target antibiotics from six common categories (β-lactams, quinolones, tetracyclines, macrolides, sulfonamides, and chloramphenicols) were selected as model compounds, and a database containing an additional 74 antibiotics was compiled for posttarget screening. The limit of detection of the target antibiotics, defined as a signal-to-noise ratio of 3, ranged from 0.04 to 1.99 ng/mL. The mean interday recoveries ranged between 79.6 and 121.3 %, with a relative standard deviation from 2.9 to 18.3 % at three spiking levels of 20 ng/mL, 50 ng/mL, and 100 ng/mL. This method was successfully applied in 60 real urine samples from schoolchildren aged 8–11 years, and four target antibiotics (azithromycin, sulfadiazine, trimethoprim, and oxytetracycline) and two posttarget antibiotics (sulfadimidine and cefaclor) were found in the urine samples. This method can be used as a large-scale biomonitoring tool for exposure of the human population to antibiotics. Graphical abstract The analysis procedure of urinary antibiotics by two-dimensional UPLC-Q/TOF MS</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-014-8197-6</identifier><identifier>PMID: 25354887</identifier><language>eng</language><publisher>Berlin/Heidelberg: Springer Berlin Heidelberg</publisher><subject>Analysis ; Analytical Chemistry ; Anti-Bacterial Agents - urine ; Antibiotics ; Azithromycin ; Biochemistry ; Biological monitoring ; Biomonitoring ; Cefaclor ; Characterization and Evaluation of Materials ; Chemical properties ; Chemistry ; Chemistry and Materials Science ; Child ; Chromatography ; Chromatography, High Pressure Liquid - economics ; Chromatography, High Pressure Liquid - instrumentation ; Chromatography, High Pressure Liquid - methods ; Contamination ; Equipment Design ; Extraction procedures ; Food Science ; Human populations ; Human wastes ; Humans ; Injection ; Ions ; Joining ; Laboratory Medicine ; Limit of Detection ; Liquid chromatography ; Mass spectrometry ; Mass Spectrometry - economics ; Mass Spectrometry - instrumentation ; Mass Spectrometry - methods ; Mass spectroscopy ; Monitoring/Environmental Analysis ; Oxytetracycline ; Quadrupoles ; Quinolones ; Sample preparation ; Scientific imaging ; Screening ; Signal to noise ratio ; Solid phases ; Spectroscopy ; Sulfadiazine ; Sulfadimidine ; Sulfonamides ; Target detection ; Tetracyclines ; Time Factors ; Time-of-flight mass spectrometry ; Trimethoprim ; Two dimensional ; Urine ; β-Lactam antibiotics</subject><ispartof>Analytical and bioanalytical chemistry, 2014-12, Vol.406 (30), p.8049-8058</ispartof><rights>Springer-Verlag Berlin Heidelberg 2014</rights><rights>COPYRIGHT 2014 Springer</rights><rights>Springer-Verlag Berlin Heidelberg 2014.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c542t-b02d2cc9120b2f91efe061beeed554e2f5b260a82b117f4198a8e366d24d8e623</citedby><cites>FETCH-LOGICAL-c542t-b02d2cc9120b2f91efe061beeed554e2f5b260a82b117f4198a8e366d24d8e623</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s00216-014-8197-6$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s00216-014-8197-6$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27924,27925,41488,42557,51319</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/25354887$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Wang, He-xing</creatorcontrib><creatorcontrib>Wang, Bin</creatorcontrib><creatorcontrib>Zhou, Ying</creatorcontrib><creatorcontrib>Jiang, Qing-wu</creatorcontrib><title>Rapid and sensitive screening and selective quantification of antibiotics in human urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><addtitle>Anal Bioanal Chem</addtitle><description>A rapid and sensitive method for the screening and selective quantification of antibiotics in urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was developed. This method allowed the injection of 200 μL urine extract. The 200-μL injection volume used in this method increased the absolute sensitivity for target antibiotics in solvent by an average 13.3 times, with a range from 8.4 to 28.5 times, compared with the 10-μL conventional injection volume. A 96-well solid phase extraction procedure was established to eliminate the contamination on the chromatographic column resulting from the large-volume injection and increase the throughput of sample preparation. Fourteen target antibiotics from six common categories (β-lactams, quinolones, tetracyclines, macrolides, sulfonamides, and chloramphenicols) were selected as model compounds, and a database containing an additional 74 antibiotics was compiled for posttarget screening. The limit of detection of the target antibiotics, defined as a signal-to-noise ratio of 3, ranged from 0.04 to 1.99 ng/mL. The mean interday recoveries ranged between 79.6 and 121.3 %, with a relative standard deviation from 2.9 to 18.3 % at three spiking levels of 20 ng/mL, 50 ng/mL, and 100 ng/mL. This method was successfully applied in 60 real urine samples from schoolchildren aged 8–11 years, and four target antibiotics (azithromycin, sulfadiazine, trimethoprim, and oxytetracycline) and two posttarget antibiotics (sulfadimidine and cefaclor) were found in the urine samples. This method can be used as a large-scale biomonitoring tool for exposure of the human population to antibiotics. Graphical abstract The analysis procedure of urinary antibiotics by two-dimensional UPLC-Q/TOF MS</description><subject>Analysis</subject><subject>Analytical Chemistry</subject><subject>Anti-Bacterial Agents - urine</subject><subject>Antibiotics</subject><subject>Azithromycin</subject><subject>Biochemistry</subject><subject>Biological monitoring</subject><subject>Biomonitoring</subject><subject>Cefaclor</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemical properties</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Child</subject><subject>Chromatography</subject><subject>Chromatography, High Pressure Liquid - economics</subject><subject>Chromatography, High Pressure Liquid - instrumentation</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Contamination</subject><subject>Equipment Design</subject><subject>Extraction procedures</subject><subject>Food Science</subject><subject>Human populations</subject><subject>Human wastes</subject><subject>Humans</subject><subject>Injection</subject><subject>Ions</subject><subject>Joining</subject><subject>Laboratory Medicine</subject><subject>Limit of Detection</subject><subject>Liquid chromatography</subject><subject>Mass spectrometry</subject><subject>Mass Spectrometry - economics</subject><subject>Mass Spectrometry - instrumentation</subject><subject>Mass Spectrometry - methods</subject><subject>Mass spectroscopy</subject><subject>Monitoring/Environmental Analysis</subject><subject>Oxytetracycline</subject><subject>Quadrupoles</subject><subject>Quinolones</subject><subject>Sample preparation</subject><subject>Scientific imaging</subject><subject>Screening</subject><subject>Signal to noise ratio</subject><subject>Solid phases</subject><subject>Spectroscopy</subject><subject>Sulfadiazine</subject><subject>Sulfadimidine</subject><subject>Sulfonamides</subject><subject>Target detection</subject><subject>Tetracyclines</subject><subject>Time Factors</subject><subject>Time-of-flight mass spectrometry</subject><subject>Trimethoprim</subject><subject>Two dimensional</subject><subject>Urine</subject><subject>β-Lactam antibiotics</subject><issn>1618-2642</issn><issn>1618-2650</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2014</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><sourceid>ABUWG</sourceid><sourceid>AFKRA</sourceid><sourceid>AZQEC</sourceid><sourceid>BENPR</sourceid><sourceid>CCPQU</sourceid><sourceid>DWQXO</sourceid><sourceid>GNUQQ</sourceid><recordid>eNqNktFuFCEUhidGY2v1AbwxJN70ZiqwwDKXTaPVpImJ0WvCMIddGgZmgbHZZ_SlZNy1jUaTZiYZ5vD9Pwf4m-Y1wRcE4_W7jDElosWEtZJ061Y8aU6JILKlguOn92NGT5oXOd9iTLgk4nlzQvmKMynXp82PL3pyA9JhQBlCdsV9B5RNAggubI51D-ZXfTfrUJx1RhcXA4oWLf-9i8WZjFxA23nUAc3JBUD9HpW72A5uXHxj0B7NviQ9QbIxVc4A8m4319XNNsVRl7ips9s9MnGePAzozpXtsuaQ5il6QKVatdG21rvNtqBR54zyVHuraihp_7J5ZrXP8Or4PWu-fXj_9epje_P5-tPV5U1rOKOl7TEdqDEdobintiNgAQvSA8DAOQNqeU8F1pL2hKwtI53UElZCDJQNEgRdnTXnB98pxd0MuajRZQPe6wBxzooI0cn6svVjUFkvi9DHuFLJqaAdqejbv9DbOKd6wllRXpsmVHT8gdpoD8oFG-vpm8VUXa46ygjDnFXq4h9UfQYYnYkBrKv1PwTkIDAp5pzAqim5Uae9IlgtsVSHWKoaS7XEUomqeXNseO5HGO4Vv3NYAXoAcp0KG0gPO_q_608IpfEX</recordid><startdate>20141201</startdate><enddate>20141201</enddate><creator>Wang, He-xing</creator><creator>Wang, Bin</creator><creator>Zhou, Ying</creator><creator>Jiang, Qing-wu</creator><general>Springer Berlin Heidelberg</general><general>Springer</general><general>Springer Nature B.V</general><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>7QF</scope><scope>7QO</scope><scope>7QQ</scope><scope>7SC</scope><scope>7SE</scope><scope>7SP</scope><scope>7SR</scope><scope>7TA</scope><scope>7TB</scope><scope>7U5</scope><scope>7U7</scope><scope>7X7</scope><scope>7XB</scope><scope>88E</scope><scope>8BQ</scope><scope>8FD</scope><scope>8FE</scope><scope>8FG</scope><scope>8FH</scope><scope>8FI</scope><scope>8FJ</scope><scope>8FK</scope><scope>ABJCF</scope><scope>ABUWG</scope><scope>AFKRA</scope><scope>AZQEC</scope><scope>BBNVY</scope><scope>BENPR</scope><scope>BGLVJ</scope><scope>BHPHI</scope><scope>C1K</scope><scope>CCPQU</scope><scope>D1I</scope><scope>DWQXO</scope><scope>F28</scope><scope>FR3</scope><scope>FYUFA</scope><scope>GHDGH</scope><scope>GNUQQ</scope><scope>H8D</scope><scope>H8G</scope><scope>HCIFZ</scope><scope>JG9</scope><scope>JQ2</scope><scope>K9.</scope><scope>KB.</scope><scope>KR7</scope><scope>L7M</scope><scope>LK8</scope><scope>L~C</scope><scope>L~D</scope><scope>M0S</scope><scope>M1P</scope><scope>M7P</scope><scope>P64</scope><scope>PDBOC</scope><scope>PQEST</scope><scope>PQQKQ</scope><scope>PQUKI</scope><scope>7X8</scope><scope>7QH</scope><scope>7TV</scope><scope>7UA</scope></search><sort><creationdate>20141201</creationdate><title>Rapid and sensitive screening and selective quantification of antibiotics in human urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry</title><author>Wang, He-xing ; Wang, Bin ; Zhou, Ying ; Jiang, Qing-wu</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c542t-b02d2cc9120b2f91efe061beeed554e2f5b260a82b117f4198a8e366d24d8e623</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2014</creationdate><topic>Analysis</topic><topic>Analytical Chemistry</topic><topic>Anti-Bacterial Agents - urine</topic><topic>Antibiotics</topic><topic>Azithromycin</topic><topic>Biochemistry</topic><topic>Biological monitoring</topic><topic>Biomonitoring</topic><topic>Cefaclor</topic><topic>Characterization and Evaluation of Materials</topic><topic>Chemical properties</topic><topic>Chemistry</topic><topic>Chemistry and Materials Science</topic><topic>Child</topic><topic>Chromatography</topic><topic>Chromatography, High Pressure Liquid - economics</topic><topic>Chromatography, High Pressure Liquid - instrumentation</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Contamination</topic><topic>Equipment Design</topic><topic>Extraction procedures</topic><topic>Food Science</topic><topic>Human populations</topic><topic>Human wastes</topic><topic>Humans</topic><topic>Injection</topic><topic>Ions</topic><topic>Joining</topic><topic>Laboratory Medicine</topic><topic>Limit of Detection</topic><topic>Liquid chromatography</topic><topic>Mass spectrometry</topic><topic>Mass Spectrometry - 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Academic</collection><collection>Aqualine</collection><collection>Pollution Abstracts</collection><collection>Water Resources Abstracts</collection><jtitle>Analytical and bioanalytical chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Wang, He-xing</au><au>Wang, Bin</au><au>Zhou, Ying</au><au>Jiang, Qing-wu</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Rapid and sensitive screening and selective quantification of antibiotics in human urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry</atitle><jtitle>Analytical and bioanalytical chemistry</jtitle><stitle>Anal Bioanal Chem</stitle><addtitle>Anal Bioanal Chem</addtitle><date>2014-12-01</date><risdate>2014</risdate><volume>406</volume><issue>30</issue><spage>8049</spage><epage>8058</epage><pages>8049-8058</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>A rapid and sensitive method for the screening and selective quantification of antibiotics in urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was developed. This method allowed the injection of 200 μL urine extract. The 200-μL injection volume used in this method increased the absolute sensitivity for target antibiotics in solvent by an average 13.3 times, with a range from 8.4 to 28.5 times, compared with the 10-μL conventional injection volume. A 96-well solid phase extraction procedure was established to eliminate the contamination on the chromatographic column resulting from the large-volume injection and increase the throughput of sample preparation. Fourteen target antibiotics from six common categories (β-lactams, quinolones, tetracyclines, macrolides, sulfonamides, and chloramphenicols) were selected as model compounds, and a database containing an additional 74 antibiotics was compiled for posttarget screening. The limit of detection of the target antibiotics, defined as a signal-to-noise ratio of 3, ranged from 0.04 to 1.99 ng/mL. The mean interday recoveries ranged between 79.6 and 121.3 %, with a relative standard deviation from 2.9 to 18.3 % at three spiking levels of 20 ng/mL, 50 ng/mL, and 100 ng/mL. This method was successfully applied in 60 real urine samples from schoolchildren aged 8–11 years, and four target antibiotics (azithromycin, sulfadiazine, trimethoprim, and oxytetracycline) and two posttarget antibiotics (sulfadimidine and cefaclor) were found in the urine samples. This method can be used as a large-scale biomonitoring tool for exposure of the human population to antibiotics. Graphical abstract The analysis procedure of urinary antibiotics by two-dimensional UPLC-Q/TOF MS</abstract><cop>Berlin/Heidelberg</cop><pub>Springer Berlin Heidelberg</pub><pmid>25354887</pmid><doi>10.1007/s00216-014-8197-6</doi><tpages>10</tpages></addata></record>
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source MEDLINE; SpringerNature Journals
subjects Analysis
Analytical Chemistry
Anti-Bacterial Agents - urine
Antibiotics
Azithromycin
Biochemistry
Biological monitoring
Biomonitoring
Cefaclor
Characterization and Evaluation of Materials
Chemical properties
Chemistry
Chemistry and Materials Science
Child
Chromatography
Chromatography, High Pressure Liquid - economics
Chromatography, High Pressure Liquid - instrumentation
Chromatography, High Pressure Liquid - methods
Contamination
Equipment Design
Extraction procedures
Food Science
Human populations
Human wastes
Humans
Injection
Ions
Joining
Laboratory Medicine
Limit of Detection
Liquid chromatography
Mass spectrometry
Mass Spectrometry - economics
Mass Spectrometry - instrumentation
Mass Spectrometry - methods
Mass spectroscopy
Monitoring/Environmental Analysis
Oxytetracycline
Quadrupoles
Quinolones
Sample preparation
Scientific imaging
Screening
Signal to noise ratio
Solid phases
Spectroscopy
Sulfadiazine
Sulfadimidine
Sulfonamides
Target detection
Tetracyclines
Time Factors
Time-of-flight mass spectrometry
Trimethoprim
Two dimensional
Urine
β-Lactam antibiotics
title Rapid and sensitive screening and selective quantification of antibiotics in human urine by two-dimensional ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry
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