Liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole and its hydrolysed and reduced metabolites in sheep muscle
A quantitative liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole, its hydrolysed metabolite and its reduced metabolite in sheep muscle has been optimised, validated and applied in a depletion study of the mebendazole-derived residues from edibl...
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| Veröffentlicht in: | Analytica chimica acta 2003-04, Vol.483 (1), p.111-123 |
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| creator | Ruyck, Hendrik De Daeseleire, Els Ridder, Herman De Renterghem, Roland Van |
| description | A quantitative liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole, its hydrolysed metabolite and its reduced metabolite in sheep muscle has been optimised, validated and applied in a depletion study of the mebendazole-derived residues from edible tissues of sheep after a single oral treatment with the commercial formulation Ovitelmin
®. The anthelmintic compounds were extracted with ethyl acetate after the sample mixture had been made alkaline. The liquid chromatographic separation was performed on a reversed phase C
18 column. Gradient elution with a mobile phase consisting of water containing 0.1% formic acid and acetonitrile was applied. Because of the detection by a very selective tandem quadrupole mass spectrometer in MS/MS mode after atmospheric pressure electrospray ionisation, the presented drug residue analysis method is very sensitive. The confirmatory method was validated according to the revised EU requirements. Most parameters were found to be conform proved to be with the criteria. The validation limit or the minimum required performance limit for sheep muscle tissue was set at 10
μg
kg
−1. The evaluated validation parameters were stability, specificity, recovery, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection capability) and applicability. The decision limit values obtained for mebendazole, the hydrolysed and the reduced metabolite were 11, 12 and 13
μg
kg
−1, respectively. The detection capabilities for these substances were 13, 15 and 16
μg
kg
−1, respectively. In the depletion study, residues of mebendazole and its two metabolites could be measured in muscle, liver, kidney as well as back fat samples. After 1 day of excretion, the residue concentrations ranged from 21 to 7630
μg
kg
−1. The highest residue concentrations were found in the liver samples. Except for the back fat samples, the highest residue values were always measured for the reduced metabolite. This substance in liver and the hydrolysed metabolite in kidney was found for 14 days after administration. |
| doi_str_mv | 10.1016/S0003-2670(02)01018-8 |
| format | Article |
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®. The anthelmintic compounds were extracted with ethyl acetate after the sample mixture had been made alkaline. The liquid chromatographic separation was performed on a reversed phase C
18 column. Gradient elution with a mobile phase consisting of water containing 0.1% formic acid and acetonitrile was applied. Because of the detection by a very selective tandem quadrupole mass spectrometer in MS/MS mode after atmospheric pressure electrospray ionisation, the presented drug residue analysis method is very sensitive. The confirmatory method was validated according to the revised EU requirements. Most parameters were found to be conform proved to be with the criteria. The validation limit or the minimum required performance limit for sheep muscle tissue was set at 10
μg
kg
−1. The evaluated validation parameters were stability, specificity, recovery, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection capability) and applicability. The decision limit values obtained for mebendazole, the hydrolysed and the reduced metabolite were 11, 12 and 13
μg
kg
−1, respectively. The detection capabilities for these substances were 13, 15 and 16
μg
kg
−1, respectively. In the depletion study, residues of mebendazole and its two metabolites could be measured in muscle, liver, kidney as well as back fat samples. After 1 day of excretion, the residue concentrations ranged from 21 to 7630
μg
kg
−1. The highest residue concentrations were found in the liver samples. Except for the back fat samples, the highest residue values were always measured for the reduced metabolite. This substance in liver and the hydrolysed metabolite in kidney was found for 14 days after administration.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/S0003-2670(02)01018-8</identifier><identifier>CODEN: ACACAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical chemistry ; Animal productions ; Biological and medical sciences ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Drug residue analysis ; Drug residue depletion ; Exact sciences and technology ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; LC–MS/MS ; Mebendazole ; Medical sciences ; Method validation ; Other chromatographic methods ; Pharmacology. Drug treatments ; Sheep muscle ; Spectrometric and optical methods ; Terrestrial animal productions ; Vertebrates</subject><ispartof>Analytica chimica acta, 2003-04, Vol.483 (1), p.111-123</ispartof><rights>2002 Elsevier Science B.V.</rights><rights>2003 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c368t-426631f3c7883185f635cdf9122d372b298da29cf861ccec7556a3738aae654d3</citedby><cites>FETCH-LOGICAL-c368t-426631f3c7883185f635cdf9122d372b298da29cf861ccec7556a3738aae654d3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/S0003-2670(02)01018-8$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>309,310,314,780,784,789,790,3550,23930,23931,25140,27924,27925,45995</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=14728081$$DView record in Pascal Francis$$Hfree_for_read</backlink></links><search><creatorcontrib>Ruyck, Hendrik De</creatorcontrib><creatorcontrib>Daeseleire, Els</creatorcontrib><creatorcontrib>Ridder, Herman De</creatorcontrib><creatorcontrib>Renterghem, Roland Van</creatorcontrib><title>Liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole and its hydrolysed and reduced metabolites in sheep muscle</title><title>Analytica chimica acta</title><description>A quantitative liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole, its hydrolysed metabolite and its reduced metabolite in sheep muscle has been optimised, validated and applied in a depletion study of the mebendazole-derived residues from edible tissues of sheep after a single oral treatment with the commercial formulation Ovitelmin
®. The anthelmintic compounds were extracted with ethyl acetate after the sample mixture had been made alkaline. The liquid chromatographic separation was performed on a reversed phase C
18 column. Gradient elution with a mobile phase consisting of water containing 0.1% formic acid and acetonitrile was applied. Because of the detection by a very selective tandem quadrupole mass spectrometer in MS/MS mode after atmospheric pressure electrospray ionisation, the presented drug residue analysis method is very sensitive. The confirmatory method was validated according to the revised EU requirements. Most parameters were found to be conform proved to be with the criteria. The validation limit or the minimum required performance limit for sheep muscle tissue was set at 10
μg
kg
−1. The evaluated validation parameters were stability, specificity, recovery, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection capability) and applicability. The decision limit values obtained for mebendazole, the hydrolysed and the reduced metabolite were 11, 12 and 13
μg
kg
−1, respectively. The detection capabilities for these substances were 13, 15 and 16
μg
kg
−1, respectively. In the depletion study, residues of mebendazole and its two metabolites could be measured in muscle, liver, kidney as well as back fat samples. After 1 day of excretion, the residue concentrations ranged from 21 to 7630
μg
kg
−1. The highest residue concentrations were found in the liver samples. Except for the back fat samples, the highest residue values were always measured for the reduced metabolite. This substance in liver and the hydrolysed metabolite in kidney was found for 14 days after administration.</description><subject>Analysis</subject><subject>Analytical chemistry</subject><subject>Animal productions</subject><subject>Biological and medical sciences</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Drug residue analysis</subject><subject>Drug residue depletion</subject><subject>Exact sciences and technology</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>LC–MS/MS</subject><subject>Mebendazole</subject><subject>Medical sciences</subject><subject>Method validation</subject><subject>Other chromatographic methods</subject><subject>Pharmacology. Drug treatments</subject><subject>Sheep muscle</subject><subject>Spectrometric and optical methods</subject><subject>Terrestrial animal productions</subject><subject>Vertebrates</subject><issn>0003-2670</issn><issn>1873-4324</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2003</creationdate><recordtype>article</recordtype><recordid>eNqFUcuqFDEQDaLgePUThGwUXbTm0Z3OrEQuvmDAhboOmaRiR9Kdvqm0MH6PH2ruzEWXrup16hR1DiFPOXvFGVevvzDGZCfUyF4w8ZK1nu70PbLjepRdL0V_n-z-Qh6SR4g_Wik463fk9yHebNFTN5U825q_F7tO0XWQwNWScS32RKtdPMx0togU1_Nghlqioy1M2dOQC60TUA8VyhwXW2NeaA5tfoTF2185AW0kNFak08mXnE4I_twq4DfX8kZljznFCkjjQnECWOm8oUvwmDwINiE8uYtX5Nv7d1-vP3aHzx8-Xb89dE4qXbteKCV5kG7UWnI9BCUH58OeC-HlKI5ir70Vexe04s6BG4dBWTlKbS2ooffyijy_8K4l32yA1cwRHaRkF8gbGj7qgWumGnC4AF2TCAsEs5Y423IynJlbT8zZE3MruGHCnD0xuu09uztg0dkUil1cxH_L_Sg007zh3lxw0L79GaEYdBGWJlMsTX7jc_zPpT8mCaTe</recordid><startdate>20030425</startdate><enddate>20030425</enddate><creator>Ruyck, Hendrik De</creator><creator>Daeseleire, Els</creator><creator>Ridder, Herman De</creator><creator>Renterghem, Roland Van</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>IQODW</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7QO</scope><scope>8FD</scope><scope>FR3</scope><scope>P64</scope></search><sort><creationdate>20030425</creationdate><title>Liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole and its hydrolysed and reduced metabolites in sheep muscle</title><author>Ruyck, Hendrik De ; Daeseleire, Els ; Ridder, Herman De ; Renterghem, Roland Van</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c368t-426631f3c7883185f635cdf9122d372b298da29cf861ccec7556a3738aae654d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2003</creationdate><topic>Analysis</topic><topic>Analytical chemistry</topic><topic>Animal productions</topic><topic>Biological and medical sciences</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Drug residue analysis</topic><topic>Drug residue depletion</topic><topic>Exact sciences and technology</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>LC–MS/MS</topic><topic>Mebendazole</topic><topic>Medical sciences</topic><topic>Method validation</topic><topic>Other chromatographic methods</topic><topic>Pharmacology. Drug treatments</topic><topic>Sheep muscle</topic><topic>Spectrometric and optical methods</topic><topic>Terrestrial animal productions</topic><topic>Vertebrates</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Ruyck, Hendrik De</creatorcontrib><creatorcontrib>Daeseleire, Els</creatorcontrib><creatorcontrib>Ridder, Herman De</creatorcontrib><creatorcontrib>Renterghem, Roland Van</creatorcontrib><collection>Pascal-Francis</collection><collection>CrossRef</collection><collection>Biotechnology Research Abstracts</collection><collection>Technology Research Database</collection><collection>Engineering Research Database</collection><collection>Biotechnology and BioEngineering Abstracts</collection><jtitle>Analytica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Ruyck, Hendrik De</au><au>Daeseleire, Els</au><au>Ridder, Herman De</au><au>Renterghem, Roland Van</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole and its hydrolysed and reduced metabolites in sheep muscle</atitle><jtitle>Analytica chimica acta</jtitle><date>2003-04-25</date><risdate>2003</risdate><volume>483</volume><issue>1</issue><spage>111</spage><epage>123</epage><pages>111-123</pages><issn>0003-2670</issn><eissn>1873-4324</eissn><coden>ACACAM</coden><abstract>A quantitative liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole, its hydrolysed metabolite and its reduced metabolite in sheep muscle has been optimised, validated and applied in a depletion study of the mebendazole-derived residues from edible tissues of sheep after a single oral treatment with the commercial formulation Ovitelmin
®. The anthelmintic compounds were extracted with ethyl acetate after the sample mixture had been made alkaline. The liquid chromatographic separation was performed on a reversed phase C
18 column. Gradient elution with a mobile phase consisting of water containing 0.1% formic acid and acetonitrile was applied. Because of the detection by a very selective tandem quadrupole mass spectrometer in MS/MS mode after atmospheric pressure electrospray ionisation, the presented drug residue analysis method is very sensitive. The confirmatory method was validated according to the revised EU requirements. Most parameters were found to be conform proved to be with the criteria. The validation limit or the minimum required performance limit for sheep muscle tissue was set at 10
μg
kg
−1. The evaluated validation parameters were stability, specificity, recovery, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection capability) and applicability. The decision limit values obtained for mebendazole, the hydrolysed and the reduced metabolite were 11, 12 and 13
μg
kg
−1, respectively. The detection capabilities for these substances were 13, 15 and 16
μg
kg
−1, respectively. In the depletion study, residues of mebendazole and its two metabolites could be measured in muscle, liver, kidney as well as back fat samples. After 1 day of excretion, the residue concentrations ranged from 21 to 7630
μg
kg
−1. The highest residue concentrations were found in the liver samples. Except for the back fat samples, the highest residue values were always measured for the reduced metabolite. This substance in liver and the hydrolysed metabolite in kidney was found for 14 days after administration.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><doi>10.1016/S0003-2670(02)01018-8</doi><tpages>13</tpages></addata></record> |
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| identifier | ISSN: 0003-2670 |
| ispartof | Analytica chimica acta, 2003-04, Vol.483 (1), p.111-123 |
| issn | 0003-2670 1873-4324 |
| language | eng |
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| source | Elsevier ScienceDirect Journals Complete |
| subjects | Analysis Analytical chemistry Animal productions Biological and medical sciences Chemistry Chromatographic methods and physical methods associated with chromatography Drug residue analysis Drug residue depletion Exact sciences and technology Fundamental and applied biological sciences. Psychology General pharmacology LC–MS/MS Mebendazole Medical sciences Method validation Other chromatographic methods Pharmacology. Drug treatments Sheep muscle Spectrometric and optical methods Terrestrial animal productions Vertebrates |
| title | Liquid chromatographic-electrospray tandem mass spectrometric method for the determination of mebendazole and its hydrolysed and reduced metabolites in sheep muscle |
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