Multitarget and suspect screening of antimicrobials in soil and manure by means of QuEChERS — liquid chromatography tandem mass spectrometry
The present work aimed to develop an accurate analytical method for the simultaneous analysis of twenty-four antimicrobials in soil:compost and animal manure samples by means of ultra-high performance liquid chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-QqQ). For this purpos...
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| creator | Vergara-Luis, I. Bocayá, N. Irazola-Duñabeitia, M. Zuloaga, O. Lacuesta, M. Olivares, M. Prieto, A. |
| description | The present work aimed to develop an accurate analytical method for the simultaneous analysis of twenty-four antimicrobials in soil:compost and animal manure samples by means of ultra-high performance liquid chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-QqQ). For this purpose, the effectiveness of two extraction techniques (i.e. focused ultrasound solid–liquid extraction (FUSLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe)) was evaluated, and the clean-up step using solid-phase extraction (SPE) was also thoroughly studied. The method was successfully validated at 10 μg·kg
−1
, 25 μg·kg
−1
, and 50 μg·kg
−1
showing adequate trueness (70–130%) and repeatability (RSD |
| doi_str_mv | 10.1007/s00216-023-04905-2 |
| format | Article |
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−1
, 25 μg·kg
−1
, and 50 μg·kg
−1
showing adequate trueness (70–130%) and repeatability (RSD < 30%), with few exceptions. Procedural limits of quantification (LOQ
PRO
) were determined for soil:compost (0.45 to 7.50 μg·kg
−1
) and manure (0.31 to 5.53 μg·kg
−1
) samples. Pefloxacin could not be validated at the lowest level since LOQ
PRO
≥ 10 μg·kg
−1
. Sulfamethazine (7.9 ± 0.8 µg·kg
−1
), danofloxacin (27.1 ± 1.4 µg·kg
−1
) and trimethoprim (4.9 ± 0.5 µg·kg
−1
) were detected in soil samples; and tetracycline (56.8 ± 2.8 µg·kg
−1
), among other antimicrobials, in the plants grown on the surface of the studied soil samples. Similarly, sulfonamides (SAs), tetracyclines (TCs) and fluoroquinolones (FQs) were detected in sheep manure in a range of 1.7 ± 0.3 to 93.3 ± 6.8 µg·kg
−1
. Soil and manure samples were also analysed through UHPLC coupled to a high-resolution mass-spectrometer (UHPLC-qOrbitrap) in order to extend the multitarget method to suspect screening of more than 22,281 suspects. A specific transformation product (TP) of sulfamethazine (formyl-sulfamethazine) was annotated at 2a level in manure samples, among others. This work contributes to the efforts that have been made in the last decade to develop analytical methods that allow multitarget analysis of a wide variety of antimicrobials, including TPs, which is a complex task due to the diverse physicochemical properties of the antimicrobials.</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-023-04905-2</identifier><identifier>PMID: 37610438</identifier><language>eng</language><publisher>Berlin/Heidelberg: Springer Berlin Heidelberg</publisher><subject>Analysis ; Analytical Chemistry ; Analytical methods ; Animal waste ; Anti-infective agents ; Antibiotics ; Antimicrobial agents ; Biochemistry ; Characterization and Evaluation of Materials ; Chemistry ; Chemistry and Materials Science ; Chromatography ; Composting ; Composts ; danofloxacin ; Fluoroquinolones ; Food Science ; High performance liquid chromatography ; Identification and classification ; Laboratory Medicine ; Liquid chromatography ; Manures ; Mass spectrometry ; Mass spectroscopy ; Methods ; Monitoring/Environmental Analysis ; Pefloxacin ; Physicochemical properties ; Quadrupoles ; Research Paper ; Screening ; Sheep manure ; soil ; Soils ; solid phase extraction ; Solid phases ; spectrometers ; Sulfamethazine ; Sulfonamides ; tandem mass spectrometry ; tetracycline ; Tetracyclines ; Trimethoprim ; ultra-performance liquid chromatography ; ultrasonics</subject><ispartof>Analytical and bioanalytical chemistry, 2023-10, Vol.415 (25), p.6291-6310</ispartof><rights>The Author(s) 2023</rights><rights>COPYRIGHT 2023 Springer</rights><rights>The Author(s) 2023. This work is published under http://creativecommons.org/licenses/by/4.0/ (the “License”). Notwithstanding the ProQuest Terms and Conditions, you may use this content in accordance with the terms of the License.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c552t-6bf848e27b7399dc774e7ba16a068eddf70bf7bdeca0cbe433ed6594607f41303</citedby><cites>FETCH-LOGICAL-c552t-6bf848e27b7399dc774e7ba16a068eddf70bf7bdeca0cbe433ed6594607f41303</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/s00216-023-04905-2$$EPDF$$P50$$Gspringer$$Hfree_for_read</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s00216-023-04905-2$$EHTML$$P50$$Gspringer$$Hfree_for_read</linktohtml><link.rule.ids>230,314,778,782,883,27907,27908,41471,42540,51302</link.rule.ids></links><search><creatorcontrib>Vergara-Luis, I.</creatorcontrib><creatorcontrib>Bocayá, N.</creatorcontrib><creatorcontrib>Irazola-Duñabeitia, M.</creatorcontrib><creatorcontrib>Zuloaga, O.</creatorcontrib><creatorcontrib>Lacuesta, M.</creatorcontrib><creatorcontrib>Olivares, M.</creatorcontrib><creatorcontrib>Prieto, A.</creatorcontrib><title>Multitarget and suspect screening of antimicrobials in soil and manure by means of QuEChERS — liquid chromatography tandem mass spectrometry</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><description>The present work aimed to develop an accurate analytical method for the simultaneous analysis of twenty-four antimicrobials in soil:compost and animal manure samples by means of ultra-high performance liquid chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-QqQ). For this purpose, the effectiveness of two extraction techniques (i.e. focused ultrasound solid–liquid extraction (FUSLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe)) was evaluated, and the clean-up step using solid-phase extraction (SPE) was also thoroughly studied. The method was successfully validated at 10 μg·kg
−1
, 25 μg·kg
−1
, and 50 μg·kg
−1
showing adequate trueness (70–130%) and repeatability (RSD < 30%), with few exceptions. Procedural limits of quantification (LOQ
PRO
) were determined for soil:compost (0.45 to 7.50 μg·kg
−1
) and manure (0.31 to 5.53 μg·kg
−1
) samples. Pefloxacin could not be validated at the lowest level since LOQ
PRO
≥ 10 μg·kg
−1
. Sulfamethazine (7.9 ± 0.8 µg·kg
−1
), danofloxacin (27.1 ± 1.4 µg·kg
−1
) and trimethoprim (4.9 ± 0.5 µg·kg
−1
) were detected in soil samples; and tetracycline (56.8 ± 2.8 µg·kg
−1
), among other antimicrobials, in the plants grown on the surface of the studied soil samples. Similarly, sulfonamides (SAs), tetracyclines (TCs) and fluoroquinolones (FQs) were detected in sheep manure in a range of 1.7 ± 0.3 to 93.3 ± 6.8 µg·kg
−1
. Soil and manure samples were also analysed through UHPLC coupled to a high-resolution mass-spectrometer (UHPLC-qOrbitrap) in order to extend the multitarget method to suspect screening of more than 22,281 suspects. A specific transformation product (TP) of sulfamethazine (formyl-sulfamethazine) was annotated at 2a level in manure samples, among others. This work contributes to the efforts that have been made in the last decade to develop analytical methods that allow multitarget analysis of a wide variety of antimicrobials, including TPs, which is a complex task due to the diverse physicochemical properties of the antimicrobials.</description><subject>Analysis</subject><subject>Analytical Chemistry</subject><subject>Analytical methods</subject><subject>Animal waste</subject><subject>Anti-infective agents</subject><subject>Antibiotics</subject><subject>Antimicrobial agents</subject><subject>Biochemistry</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Chromatography</subject><subject>Composting</subject><subject>Composts</subject><subject>danofloxacin</subject><subject>Fluoroquinolones</subject><subject>Food Science</subject><subject>High performance liquid chromatography</subject><subject>Identification and classification</subject><subject>Laboratory Medicine</subject><subject>Liquid chromatography</subject><subject>Manures</subject><subject>Mass spectrometry</subject><subject>Mass spectroscopy</subject><subject>Methods</subject><subject>Monitoring/Environmental Analysis</subject><subject>Pefloxacin</subject><subject>Physicochemical properties</subject><subject>Quadrupoles</subject><subject>Research Paper</subject><subject>Screening</subject><subject>Sheep manure</subject><subject>soil</subject><subject>Soils</subject><subject>solid phase extraction</subject><subject>Solid phases</subject><subject>spectrometers</subject><subject>Sulfamethazine</subject><subject>Sulfonamides</subject><subject>tandem mass spectrometry</subject><subject>tetracycline</subject><subject>Tetracyclines</subject><subject>Trimethoprim</subject><subject>ultra-performance liquid 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and suspect screening of antimicrobials in soil and manure by means of QuEChERS — liquid chromatography tandem mass spectrometry</title><author>Vergara-Luis, I. ; Bocayá, N. ; Irazola-Duñabeitia, M. ; Zuloaga, O. ; Lacuesta, M. ; Olivares, M. ; Prieto, A.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c552t-6bf848e27b7399dc774e7ba16a068eddf70bf7bdeca0cbe433ed6594607f41303</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2023</creationdate><topic>Analysis</topic><topic>Analytical Chemistry</topic><topic>Analytical methods</topic><topic>Animal waste</topic><topic>Anti-infective agents</topic><topic>Antibiotics</topic><topic>Antimicrobial agents</topic><topic>Biochemistry</topic><topic>Characterization and Evaluation of Materials</topic><topic>Chemistry</topic><topic>Chemistry and Materials 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spectrometry</atitle><jtitle>Analytical and bioanalytical chemistry</jtitle><stitle>Anal Bioanal Chem</stitle><date>2023-10-01</date><risdate>2023</risdate><volume>415</volume><issue>25</issue><spage>6291</spage><epage>6310</epage><pages>6291-6310</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>The present work aimed to develop an accurate analytical method for the simultaneous analysis of twenty-four antimicrobials in soil:compost and animal manure samples by means of ultra-high performance liquid chromatography coupled to a triple-quadrupole mass spectrometer (UHPLC-QqQ). For this purpose, the effectiveness of two extraction techniques (i.e. focused ultrasound solid–liquid extraction (FUSLE) and QuEChERS (quick, easy, cheap, effective, rugged and safe)) was evaluated, and the clean-up step using solid-phase extraction (SPE) was also thoroughly studied. The method was successfully validated at 10 μg·kg
−1
, 25 μg·kg
−1
, and 50 μg·kg
−1
showing adequate trueness (70–130%) and repeatability (RSD < 30%), with few exceptions. Procedural limits of quantification (LOQ
PRO
) were determined for soil:compost (0.45 to 7.50 μg·kg
−1
) and manure (0.31 to 5.53 μg·kg
−1
) samples. Pefloxacin could not be validated at the lowest level since LOQ
PRO
≥ 10 μg·kg
−1
. Sulfamethazine (7.9 ± 0.8 µg·kg
−1
), danofloxacin (27.1 ± 1.4 µg·kg
−1
) and trimethoprim (4.9 ± 0.5 µg·kg
−1
) were detected in soil samples; and tetracycline (56.8 ± 2.8 µg·kg
−1
), among other antimicrobials, in the plants grown on the surface of the studied soil samples. Similarly, sulfonamides (SAs), tetracyclines (TCs) and fluoroquinolones (FQs) were detected in sheep manure in a range of 1.7 ± 0.3 to 93.3 ± 6.8 µg·kg
−1
. Soil and manure samples were also analysed through UHPLC coupled to a high-resolution mass-spectrometer (UHPLC-qOrbitrap) in order to extend the multitarget method to suspect screening of more than 22,281 suspects. A specific transformation product (TP) of sulfamethazine (formyl-sulfamethazine) was annotated at 2a level in manure samples, among others. This work contributes to the efforts that have been made in the last decade to develop analytical methods that allow multitarget analysis of a wide variety of antimicrobials, including TPs, which is a complex task due to the diverse physicochemical properties of the antimicrobials.</abstract><cop>Berlin/Heidelberg</cop><pub>Springer Berlin Heidelberg</pub><pmid>37610438</pmid><doi>10.1007/s00216-023-04905-2</doi><tpages>20</tpages><oa>free_for_read</oa></addata></record> |
| fulltext | fulltext |
| identifier | ISSN: 1618-2642 |
| ispartof | Analytical and bioanalytical chemistry, 2023-10, Vol.415 (25), p.6291-6310 |
| issn | 1618-2642 1618-2650 |
| language | eng |
| recordid | cdi_pubmedcentral_primary_oai_pubmedcentral_nih_gov_10558387 |
| source | SpringerLink Journals |
| subjects | Analysis Analytical Chemistry Analytical methods Animal waste Anti-infective agents Antibiotics Antimicrobial agents Biochemistry Characterization and Evaluation of Materials Chemistry Chemistry and Materials Science Chromatography Composting Composts danofloxacin Fluoroquinolones Food Science High performance liquid chromatography Identification and classification Laboratory Medicine Liquid chromatography Manures Mass spectrometry Mass spectroscopy Methods Monitoring/Environmental Analysis Pefloxacin Physicochemical properties Quadrupoles Research Paper Screening Sheep manure soil Soils solid phase extraction Solid phases spectrometers Sulfamethazine Sulfonamides tandem mass spectrometry tetracycline Tetracyclines Trimethoprim ultra-performance liquid chromatography ultrasonics |
| title | Multitarget and suspect screening of antimicrobials in soil and manure by means of QuEChERS — liquid chromatography tandem mass spectrometry |
| url | https://sfx.bib-bvb.de/sfx_tum?ctx_ver=Z39.88-2004&ctx_enc=info:ofi/enc:UTF-8&ctx_tim=2025-01-16T19%3A56%3A07IST&url_ver=Z39.88-2004&url_ctx_fmt=infofi/fmt:kev:mtx:ctx&rfr_id=info:sid/primo.exlibrisgroup.com:primo3-Article-gale_pubme&rft_val_fmt=info:ofi/fmt:kev:mtx:journal&rft.genre=article&rft.atitle=Multitarget%20and%20suspect%20screening%20of%20antimicrobials%20in%20soil%20and%20manure%20by%20means%20of%20QuEChERS%20%E2%80%94%20liquid%20chromatography%20tandem%20mass%20spectrometry&rft.jtitle=Analytical%20and%20bioanalytical%20chemistry&rft.au=Vergara-Luis,%20I.&rft.date=2023-10-01&rft.volume=415&rft.issue=25&rft.spage=6291&rft.epage=6310&rft.pages=6291-6310&rft.issn=1618-2642&rft.eissn=1618-2650&rft_id=info:doi/10.1007/s00216-023-04905-2&rft_dat=%3Cgale_pubme%3EA768047914%3C/gale_pubme%3E%3Curl%3E%3C/url%3E&disable_directlink=true&sfx.directlink=off&sfx.report_link=0&rft_id=info:oai/&rft_pqid=2873636524&rft_id=info:pmid/37610438&rft_galeid=A768047914&rfr_iscdi=true |