Development and validation of a rapid, sensitive liquid chromatography–tandem mass spectrometry method using electrospray ionization for quantitation of centchroman in rat plasma and its application to preclinical pharmacokinetic study
A highly sensitive and specific HPLC–ESI-MS/MS method has been developed and validated for the estimation of centchroman with 100 μL rat plasma using tamoxifen as an internal standard (IS). The assay procedure involved a single-step, liquid–liquid extraction of centchroman and IS from plasma with 2....
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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, 2008-12, Vol.876 (1), p.1-7 |
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creator | Singh, Sheelendra Pratap Singh, Ravi Shankar Prasad Wahajuddin Jain, Girish Kumar |
description | A highly sensitive and specific HPLC–ESI-MS/MS method has been developed and validated for the estimation of centchroman with 100
μL rat plasma using tamoxifen as an internal standard (IS). The assay procedure involved a single-step, liquid–liquid extraction of centchroman and IS from plasma with 2.5% (v/v) isopropanol in
n-hexane, which yielded consistent recoveries of 109.5 and 107.8% for centchroman and IS in rat plasma, respectively. The total chromatographic run time was 3.8
min. Peaks were resolved using 0.01
M ammonium acetate (pH 4.5):acetonitrile (10:90, v/v) mobile phase on a Supelco Discovery C
18 column. Specificity and matrix effect on ionization was determined and found that method was specific and there was no significant matrix effect. Linearity range was found to be 0.5–100.0
ng/mL with a correlation coefficient (
r) of 0.9959 or better. The intra- and inter-day assay precision ranged from 3.3 to 9.0% and 5.5 to 6.8%, respectively, and intra- and inter-day assay accuracy was between 93.4–107.1% and 96.2–104.2%, respectively. Stability of centchroman in rat plasma was >89.0% in the battery of stability studies viz., bench-top, auto-sampler, freeze/thaw cycles and 30 days storage in a freezer at −80
°C. The assay was successfully applied to determine the pharmacokinetic parameters in
Sprague–
Dawley rats after an oral administration of centchroman at 20
mg/kg. As a result, the plasma half-life was 29.4
±
2.3
h and the AUC
(0–∞) was 7345.1
±
21.9
ng
h/mL. The maximum plasma concentration (
C
max) 117.5
±
15.7
ng/mL was achieved at 9.0
±
8.6
h (
t
max). |
doi_str_mv | 10.1016/j.jchromb.2008.09.039 |
format | Article |
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μL rat plasma using tamoxifen as an internal standard (IS). The assay procedure involved a single-step, liquid–liquid extraction of centchroman and IS from plasma with 2.5% (v/v) isopropanol in
n-hexane, which yielded consistent recoveries of 109.5 and 107.8% for centchroman and IS in rat plasma, respectively. The total chromatographic run time was 3.8
min. Peaks were resolved using 0.01
M ammonium acetate (pH 4.5):acetonitrile (10:90, v/v) mobile phase on a Supelco Discovery C
18 column. Specificity and matrix effect on ionization was determined and found that method was specific and there was no significant matrix effect. Linearity range was found to be 0.5–100.0
ng/mL with a correlation coefficient (
r) of 0.9959 or better. The intra- and inter-day assay precision ranged from 3.3 to 9.0% and 5.5 to 6.8%, respectively, and intra- and inter-day assay accuracy was between 93.4–107.1% and 96.2–104.2%, respectively. Stability of centchroman in rat plasma was >89.0% in the battery of stability studies viz., bench-top, auto-sampler, freeze/thaw cycles and 30 days storage in a freezer at −80
°C. The assay was successfully applied to determine the pharmacokinetic parameters in
Sprague–
Dawley rats after an oral administration of centchroman at 20
mg/kg. As a result, the plasma half-life was 29.4
±
2.3
h and the AUC
(0–∞) was 7345.1
±
21.9
ng
h/mL. The maximum plasma concentration (
C
max) 117.5
±
15.7
ng/mL was achieved at 9.0
±
8.6
h (
t
max).</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2008.09.039</identifier><identifier>PMID: 19004674</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical, structural and metabolic biochemistry ; Animals ; Biological and medical sciences ; Centchroman ; Centchroman - blood ; Centchroman - pharmacokinetics ; Chromatography, High Pressure Liquid - methods ; Drug Stability ; Female ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; LC–MS/MS ; Medical sciences ; Pharmacokinetics ; Pharmacology. Drug treatments ; Rat plasma ; Rats ; Rats, Sprague-Dawley ; Reproducibility of Results ; Sensitivity and Specificity ; Spectrometry, Mass, Electrospray Ionization - methods ; Tandem Mass Spectrometry - methods ; Validation</subject><ispartof>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2008-12, Vol.876 (1), p.1-7</ispartof><rights>2008 Elsevier B.V.</rights><rights>2009 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c422t-31bdf32c7268b397d41048f0d43dd3c1475db05a59084fd7f9918a681c6ccbca3</citedby><cites>FETCH-LOGICAL-c422t-31bdf32c7268b397d41048f0d43dd3c1475db05a59084fd7f9918a681c6ccbca3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S1570023208007289$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27903,27904,65309</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=20951746$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/19004674$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Singh, Sheelendra Pratap</creatorcontrib><creatorcontrib>Singh, Ravi Shankar Prasad</creatorcontrib><creatorcontrib>Wahajuddin</creatorcontrib><creatorcontrib>Jain, Girish Kumar</creatorcontrib><title>Development and validation of a rapid, sensitive liquid chromatography–tandem mass spectrometry method using electrospray ionization for quantitation of centchroman in rat plasma and its application to preclinical pharmacokinetic study</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 highly sensitive and specific HPLC–ESI-MS/MS method has been developed and validated for the estimation of centchroman with 100
μL rat plasma using tamoxifen as an internal standard (IS). The assay procedure involved a single-step, liquid–liquid extraction of centchroman and IS from plasma with 2.5% (v/v) isopropanol in
n-hexane, which yielded consistent recoveries of 109.5 and 107.8% for centchroman and IS in rat plasma, respectively. The total chromatographic run time was 3.8
min. Peaks were resolved using 0.01
M ammonium acetate (pH 4.5):acetonitrile (10:90, v/v) mobile phase on a Supelco Discovery C
18 column. Specificity and matrix effect on ionization was determined and found that method was specific and there was no significant matrix effect. Linearity range was found to be 0.5–100.0
ng/mL with a correlation coefficient (
r) of 0.9959 or better. The intra- and inter-day assay precision ranged from 3.3 to 9.0% and 5.5 to 6.8%, respectively, and intra- and inter-day assay accuracy was between 93.4–107.1% and 96.2–104.2%, respectively. Stability of centchroman in rat plasma was >89.0% in the battery of stability studies viz., bench-top, auto-sampler, freeze/thaw cycles and 30 days storage in a freezer at −80
°C. The assay was successfully applied to determine the pharmacokinetic parameters in
Sprague–
Dawley rats after an oral administration of centchroman at 20
mg/kg. As a result, the plasma half-life was 29.4
±
2.3
h and the AUC
(0–∞) was 7345.1
±
21.9
ng
h/mL. The maximum plasma concentration (
C
max) 117.5
±
15.7
ng/mL was achieved at 9.0
±
8.6
h (
t
max).</description><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Animals</subject><subject>Biological and medical sciences</subject><subject>Centchroman</subject><subject>Centchroman - blood</subject><subject>Centchroman - pharmacokinetics</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Drug Stability</subject><subject>Female</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>LC–MS/MS</subject><subject>Medical sciences</subject><subject>Pharmacokinetics</subject><subject>Pharmacology. Drug treatments</subject><subject>Rat plasma</subject><subject>Rats</subject><subject>Rats, Sprague-Dawley</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Validation</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>eNqFUc2OFCEY7BiNu64-goaLnpwRmu6mORmzrj_JJl408UZooHe-kQYG6EnG076Db-jdd5CdnqxHL0D4qr6qVFXVc4LXBJPuzXa9VZvop2FdY9yvMV9jyh9U56RndEVZ9_1hebcMr3BN67PqSUpbjAnDjD6uzgjHuOlYc179eW_2xvowGZeRdBrtpQUtM3iH_IgkijKAfo2ScQky7A2ysJtBo6O4zP6mADaH37e_cmGbCU0yJZSCUbnMTY4HVM6N12hO4G6QscdJClEeUBGBn4vW6CPazdJlyPfiqnhaZBwCV5xkFKxMkzwahZyQDMGCWgjZoxCNsuDKj0VhI-Mklf8BzmRQKOVZH55Wj0Zpk3l2ui-qbx-uvl5-Wl1_-fj58t31SjV1nVeUDHqktWJ11w-UM90Q3PQj1g3VmirSsFYPuJUtx30zajZyTnrZ9UR1Sg1K0ovq1bI3RL-bTcpigqSMtdIZPyfR8b6sbngBtgtQlUxSNKMIESYZD4Jgcdez2IpTz-KuZ4G5KD0X3ouTwDxMRv9jnYotgJcngEwljjFKpyDd42rMW8KaruDeLjhT4tiDiSIpME4ZDSXMLLSH_1j5C-6U03E</recordid><startdate>20081201</startdate><enddate>20081201</enddate><creator>Singh, Sheelendra Pratap</creator><creator>Singh, Ravi Shankar Prasad</creator><creator>Wahajuddin</creator><creator>Jain, Girish Kumar</creator><general>Elsevier B.V</general><general>Elsevier</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>20081201</creationdate><title>Development and validation of a rapid, sensitive liquid chromatography–tandem mass spectrometry method using electrospray ionization for quantitation of centchroman in rat plasma and its application to preclinical pharmacokinetic study</title><author>Singh, Sheelendra Pratap ; Singh, Ravi Shankar Prasad ; Wahajuddin ; Jain, Girish Kumar</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c422t-31bdf32c7268b397d41048f0d43dd3c1475db05a59084fd7f9918a681c6ccbca3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2008</creationdate><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Animals</topic><topic>Biological and medical sciences</topic><topic>Centchroman</topic><topic>Centchroman - blood</topic><topic>Centchroman - pharmacokinetics</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Drug Stability</topic><topic>Female</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>LC–MS/MS</topic><topic>Medical sciences</topic><topic>Pharmacokinetics</topic><topic>Pharmacology. Drug treatments</topic><topic>Rat plasma</topic><topic>Rats</topic><topic>Rats, Sprague-Dawley</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Validation</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Singh, Sheelendra Pratap</creatorcontrib><creatorcontrib>Singh, Ravi Shankar Prasad</creatorcontrib><creatorcontrib>Wahajuddin</creatorcontrib><creatorcontrib>Jain, Girish Kumar</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>Singh, Sheelendra Pratap</au><au>Singh, Ravi Shankar Prasad</au><au>Wahajuddin</au><au>Jain, Girish Kumar</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Development and validation of a rapid, sensitive liquid chromatography–tandem mass spectrometry method using electrospray ionization for quantitation of centchroman in rat plasma and its application to preclinical pharmacokinetic study</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>2008-12-01</date><risdate>2008</risdate><volume>876</volume><issue>1</issue><spage>1</spage><epage>7</epage><pages>1-7</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>A highly sensitive and specific HPLC–ESI-MS/MS method has been developed and validated for the estimation of centchroman with 100
μL rat plasma using tamoxifen as an internal standard (IS). The assay procedure involved a single-step, liquid–liquid extraction of centchroman and IS from plasma with 2.5% (v/v) isopropanol in
n-hexane, which yielded consistent recoveries of 109.5 and 107.8% for centchroman and IS in rat plasma, respectively. The total chromatographic run time was 3.8
min. Peaks were resolved using 0.01
M ammonium acetate (pH 4.5):acetonitrile (10:90, v/v) mobile phase on a Supelco Discovery C
18 column. Specificity and matrix effect on ionization was determined and found that method was specific and there was no significant matrix effect. Linearity range was found to be 0.5–100.0
ng/mL with a correlation coefficient (
r) of 0.9959 or better. The intra- and inter-day assay precision ranged from 3.3 to 9.0% and 5.5 to 6.8%, respectively, and intra- and inter-day assay accuracy was between 93.4–107.1% and 96.2–104.2%, respectively. Stability of centchroman in rat plasma was >89.0% in the battery of stability studies viz., bench-top, auto-sampler, freeze/thaw cycles and 30 days storage in a freezer at −80
°C. The assay was successfully applied to determine the pharmacokinetic parameters in
Sprague–
Dawley rats after an oral administration of centchroman at 20
mg/kg. As a result, the plasma half-life was 29.4
±
2.3
h and the AUC
(0–∞) was 7345.1
±
21.9
ng
h/mL. The maximum plasma concentration (
C
max) 117.5
±
15.7
ng/mL was achieved at 9.0
±
8.6
h (
t
max).</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>19004674</pmid><doi>10.1016/j.jchromb.2008.09.039</doi><tpages>7</tpages></addata></record> |
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source | MEDLINE; Elsevier ScienceDirect Journals |
subjects | Analysis Analytical, structural and metabolic biochemistry Animals Biological and medical sciences Centchroman Centchroman - blood Centchroman - pharmacokinetics Chromatography, High Pressure Liquid - methods Drug Stability Female Fundamental and applied biological sciences. Psychology General pharmacology LC–MS/MS Medical sciences Pharmacokinetics Pharmacology. Drug treatments Rat plasma Rats Rats, Sprague-Dawley Reproducibility of Results Sensitivity and Specificity Spectrometry, Mass, Electrospray Ionization - methods Tandem Mass Spectrometry - methods Validation |
title | Development and validation of a rapid, sensitive liquid chromatography–tandem mass spectrometry method using electrospray ionization for quantitation of centchroman in rat plasma and its application to preclinical pharmacokinetic study |
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