Pharmacokinetics and metabolism study of firocoxib in camels after intravenous administration by using high-resolution bench-top orbitrap mass spectrometry

•A method to quantify firocoxib by high-resolution orbitrap mass spectrometry.•Method validated with excellent recovery, linearity, precision and accuracy.•Method was successfully utilized for firocoxib pharmacokinetic analysis in camels.•The method was used to tentatively identify firocoxib metabol...

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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, 2015-01, Vol.974, p.17-23
Hauptverfasser: Wasfi, Ibrahim A., Saeed, Hanan M., Agha, B.A., Kamel, Asmaa M., Biriki, Nasreen A. Al, Neaimi, Khaled M. Al, Ali, Waleed A. Al, Sultan, Saeed Mahmoud
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container_title Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
container_volume 974
creator Wasfi, Ibrahim A.
Saeed, Hanan M.
Agha, B.A.
Kamel, Asmaa M.
Biriki, Nasreen A. Al
Neaimi, Khaled M. Al
Ali, Waleed A. Al
Sultan, Saeed Mahmoud
description •A method to quantify firocoxib by high-resolution orbitrap mass spectrometry.•Method validated with excellent recovery, linearity, precision and accuracy.•Method was successfully utilized for firocoxib pharmacokinetic analysis in camels.•The method was used to tentatively identify firocoxib metabolite in camel plasma. In this study, we developed a high-resolution liquid chromatography mass spectrometry method for the pharmacokinetic study of firocoxib followed by full method validation. Following a solid-phase extraction, the firocoxib and internal standard (celecoxib) were separated on an Agilent Zorbax ZDB C18 column (50mm×2.1mm i.d., 3.5μm) with a gradient elution using methanol and 0.1% aqueous formic acid. Data acquisition was performed at 25,000 resolution with the automatic gain set to 1,000,000 and the maximum injection time of 100ms. Data were acquired in full-scan mode over a mass range of 100–550Da in positive electrospray mode. Linear calibration curves were obtained over the concentration ranges of 0.5–200ng/mL and no interfering peaks were detected at the retention time of firocoxib and internal standard in blank camel plasma samples. The mean extraction recoveries of firocoxib at three concentrations of 5, 25 and 75ng/mL ranged from 92 to 104%. Coefficient of variation of intra-day and inter-day precision were both
doi_str_mv 10.1016/j.jchromb.2014.10.021
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Following a solid-phase extraction, the firocoxib and internal standard (celecoxib) were separated on an Agilent Zorbax ZDB C18 column (50mm×2.1mm i.d., 3.5μm) with a gradient elution using methanol and 0.1% aqueous formic acid. Data acquisition was performed at 25,000 resolution with the automatic gain set to 1,000,000 and the maximum injection time of 100ms. Data were acquired in full-scan mode over a mass range of 100–550Da in positive electrospray mode. Linear calibration curves were obtained over the concentration ranges of 0.5–200ng/mL and no interfering peaks were detected at the retention time of firocoxib and internal standard in blank camel plasma samples. The mean extraction recoveries of firocoxib at three concentrations of 5, 25 and 75ng/mL ranged from 92 to 104%. Coefficient of variation of intra-day and inter-day precision were both &lt;10%. The accuracy of the method ranged from 95 to 107%. The validated method was then successfully applied in evaluating the pharmacokinetics and metabolism of firocoxib in camels (Camelus dromedarus) (n=5) following intravenous (i.v.) administration of a dose of 0.1mgkg/body weight. The results obtained (mean±SD) were as follows: the terminal elimination half-life (t1/2β) was 5.75±2.26h, and total body clearance (ClT) was 354.1±82.6mL/kg/h. The volume of distribution at steady state (VSS) was 2344.4±238.7mL/kg. One metabolite of firocoxib was tentatively identified as desalkyl firocoxib (m/z 283). 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Al</creatorcontrib><creatorcontrib>Neaimi, Khaled M. Al</creatorcontrib><creatorcontrib>Ali, Waleed A. Al</creatorcontrib><creatorcontrib>Sultan, Saeed Mahmoud</creatorcontrib><title>Pharmacokinetics and metabolism study of firocoxib in camels after intravenous administration by using high-resolution bench-top orbitrap mass spectrometry</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 method to quantify firocoxib by high-resolution orbitrap mass spectrometry.•Method validated with excellent recovery, linearity, precision and accuracy.•Method was successfully utilized for firocoxib pharmacokinetic analysis in camels.•The method was used to tentatively identify firocoxib metabolite in camel plasma. In this study, we developed a high-resolution liquid chromatography mass spectrometry method for the pharmacokinetic study of firocoxib followed by full method validation. Following a solid-phase extraction, the firocoxib and internal standard (celecoxib) were separated on an Agilent Zorbax ZDB C18 column (50mm×2.1mm i.d., 3.5μm) with a gradient elution using methanol and 0.1% aqueous formic acid. Data acquisition was performed at 25,000 resolution with the automatic gain set to 1,000,000 and the maximum injection time of 100ms. Data were acquired in full-scan mode over a mass range of 100–550Da in positive electrospray mode. Linear calibration curves were obtained over the concentration ranges of 0.5–200ng/mL and no interfering peaks were detected at the retention time of firocoxib and internal standard in blank camel plasma samples. The mean extraction recoveries of firocoxib at three concentrations of 5, 25 and 75ng/mL ranged from 92 to 104%. Coefficient of variation of intra-day and inter-day precision were both &lt;10%. The accuracy of the method ranged from 95 to 107%. The validated method was then successfully applied in evaluating the pharmacokinetics and metabolism of firocoxib in camels (Camelus dromedarus) (n=5) following intravenous (i.v.) administration of a dose of 0.1mgkg/body weight. The results obtained (mean±SD) were as follows: the terminal elimination half-life (t1/2β) was 5.75±2.26h, and total body clearance (ClT) was 354.1±82.6mL/kg/h. The volume of distribution at steady state (VSS) was 2344.4±238.7mL/kg. One metabolite of firocoxib was tentatively identified as desalkyl firocoxib (m/z 283). Firocoxib could be detected in plasma 3–5 days following i.v. administration in camels using a sensitive liquid chromatography high-resolution orbitrap mass spectrometry method.</description><subject>4-Butyrolactone - administration &amp; dosage</subject><subject>4-Butyrolactone - analogs &amp; derivatives</subject><subject>4-Butyrolactone - metabolism</subject><subject>4-Butyrolactone - pharmacokinetics</subject><subject>Administration, Intravenous</subject><subject>Animals</subject><subject>Automation</subject><subject>Camels</subject><subject>Camelus - metabolism</subject><subject>Clearance</subject><subject>Extraction</subject><subject>Firocoxib</subject><subject>High resolution</subject><subject>Liquid chromatography</subject><subject>Mass spectrometry</subject><subject>Mass Spectrometry - instrumentation</subject><subject>Mass Spectrometry - methods</subject><subject>Metabolism</subject><subject>Methyl alcohol</subject><subject>Orbitrap</subject><subject>Pharmacokinetics</subject><subject>Sulfones - administration &amp; dosage</subject><subject>Sulfones - metabolism</subject><subject>Sulfones - pharmacokinetics</subject><issn>1570-0232</issn><issn>1873-376X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2015</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkc1u1DAUhS0EoqXwCCAv2WTwTxLHK4QqfipVggVI7CzHvmk8xHawnYp5Fl4Wj2botiv7Hn_XV_cchF5TsqOE9u_2u72ZU_TjjhHaVm1HGH2CLukgeMNF__NpvXeCNIRxdoFe5LwnhAoi-HN0wbq251TyS_T326yT1yb-cgGKMxnrYLGHose4uOxxLps94DjhyaVo4h83Yhew0R6Wyk4FUq1L0vcQ4lYV611wuQrFxYDHA96yC3d4dndzkyDHZTs9QDBzU-KKYxpdxVfsdc44r2BKXQtKOrxEzya9ZHh1Pq_Qj08fv19_aW6_fr65_nDbGC6H0mhtCRFyHLSWA3S8kx1re-gnbThtbUfF0Apba8pHpsFazaUWk2x5z6RkE79Cb0__rin-3iAX5V02sCw6QN1J0b6jXMihOvs4ymUrB066inYn1KSYc4JJrcl5nQ6KEnWMUO3VOUJ1jPAo1whr35vziG30YB-6_mdWgfcnoCYA9w6SysZVO8G6VM1TNrpHRvwDWc20ag</recordid><startdate>20150101</startdate><enddate>20150101</enddate><creator>Wasfi, Ibrahim A.</creator><creator>Saeed, Hanan M.</creator><creator>Agha, B.A.</creator><creator>Kamel, Asmaa M.</creator><creator>Biriki, Nasreen A. Al</creator><creator>Neaimi, Khaled M. Al</creator><creator>Ali, Waleed A. Al</creator><creator>Sultan, Saeed Mahmoud</creator><general>Elsevier 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>7X8</scope><scope>7TB</scope><scope>8FD</scope><scope>FR3</scope></search><sort><creationdate>20150101</creationdate><title>Pharmacokinetics and metabolism study of firocoxib in camels after intravenous administration by using high-resolution bench-top orbitrap mass spectrometry</title><author>Wasfi, Ibrahim A. ; Saeed, Hanan M. ; Agha, B.A. ; Kamel, Asmaa M. ; Biriki, Nasreen A. Al ; Neaimi, Khaled M. Al ; Ali, Waleed A. 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Al</au><au>Neaimi, Khaled M. Al</au><au>Ali, Waleed A. Al</au><au>Sultan, Saeed Mahmoud</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Pharmacokinetics and metabolism study of firocoxib in camels after intravenous administration by using high-resolution bench-top orbitrap mass spectrometry</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>2015-01-01</date><risdate>2015</risdate><volume>974</volume><spage>17</spage><epage>23</epage><pages>17-23</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>•A method to quantify firocoxib by high-resolution orbitrap mass spectrometry.•Method validated with excellent recovery, linearity, precision and accuracy.•Method was successfully utilized for firocoxib pharmacokinetic analysis in camels.•The method was used to tentatively identify firocoxib metabolite in camel plasma. In this study, we developed a high-resolution liquid chromatography mass spectrometry method for the pharmacokinetic study of firocoxib followed by full method validation. Following a solid-phase extraction, the firocoxib and internal standard (celecoxib) were separated on an Agilent Zorbax ZDB C18 column (50mm×2.1mm i.d., 3.5μm) with a gradient elution using methanol and 0.1% aqueous formic acid. Data acquisition was performed at 25,000 resolution with the automatic gain set to 1,000,000 and the maximum injection time of 100ms. Data were acquired in full-scan mode over a mass range of 100–550Da in positive electrospray mode. Linear calibration curves were obtained over the concentration ranges of 0.5–200ng/mL and no interfering peaks were detected at the retention time of firocoxib and internal standard in blank camel plasma samples. The mean extraction recoveries of firocoxib at three concentrations of 5, 25 and 75ng/mL ranged from 92 to 104%. Coefficient of variation of intra-day and inter-day precision were both &lt;10%. The accuracy of the method ranged from 95 to 107%. The validated method was then successfully applied in evaluating the pharmacokinetics and metabolism of firocoxib in camels (Camelus dromedarus) (n=5) following intravenous (i.v.) administration of a dose of 0.1mgkg/body weight. The results obtained (mean±SD) were as follows: the terminal elimination half-life (t1/2β) was 5.75±2.26h, and total body clearance (ClT) was 354.1±82.6mL/kg/h. The volume of distribution at steady state (VSS) was 2344.4±238.7mL/kg. One metabolite of firocoxib was tentatively identified as desalkyl firocoxib (m/z 283). Firocoxib could be detected in plasma 3–5 days following i.v. administration in camels using a sensitive liquid chromatography high-resolution orbitrap mass spectrometry method.</abstract><cop>Netherlands</cop><pub>Elsevier B.V</pub><pmid>25463193</pmid><doi>10.1016/j.jchromb.2014.10.021</doi><tpages>7</tpages></addata></record>
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1873-376X
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source MEDLINE; Elsevier ScienceDirect Journals
subjects 4-Butyrolactone - administration & dosage
4-Butyrolactone - analogs & derivatives
4-Butyrolactone - metabolism
4-Butyrolactone - pharmacokinetics
Administration, Intravenous
Animals
Automation
Camels
Camelus - metabolism
Clearance
Extraction
Firocoxib
High resolution
Liquid chromatography
Mass spectrometry
Mass Spectrometry - instrumentation
Mass Spectrometry - methods
Metabolism
Methyl alcohol
Orbitrap
Pharmacokinetics
Sulfones - administration & dosage
Sulfones - metabolism
Sulfones - pharmacokinetics
title Pharmacokinetics and metabolism study of firocoxib in camels after intravenous administration by using high-resolution bench-top orbitrap mass spectrometry
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