HPLC-PDA-ORD Bioassay of S-(+) and R-(−) Clopidogrel on Rat Dried Blood Spots
ABSTRACT A simple and rapid chiral high‐performance liquid chromatography (HPLC) method was developed and validated for bioanalysis of clopidogrel enantiomers on rat dried blood spots (DBS). Clopidogrel enantiomers were extracted from DBS using ethanol: methanol (80:20, v/v) and separated on a Chira...
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| Veröffentlicht in: | Chirality (New York, N.Y.) N.Y.), 2014-02, Vol.26 (2), p.102-107 |
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| creator | Nageswara Rao, Ramisetti Prasad, Katuri Guru Bindu Priya, Pullakandam Bijarji, Shriharsh |
| description | ABSTRACT
A simple and rapid chiral high‐performance liquid chromatography (HPLC) method was developed and validated for bioanalysis of clopidogrel enantiomers on rat dried blood spots (DBS). Clopidogrel enantiomers were extracted from DBS using ethanol: methanol (80:20, v/v) and separated on a Chiralcel OJ‐H column containing cellulose tris (4‐methly benzoate) as a polysaccharide stationary phase using n‐hexane–ethanol‐diethylamine (70:30, 0.1 v/v) as a mobile phase at a flow rate of 1.0 mL/min. The detection was carried out at 220 nm using a photodiode array (PDA) detector while the elution order of the enantiomers was determined by a polarimeter connected to PDA in series. The effect of hematocrit on extraction of clopidogrel enantiomers from DBS was evaluated and no interference from endogenous substances was noticed. The overall accuracy of (R) and (S) enantiomers of clopidogrel from DBS were 91.6 and 89.2%, respectively. The calibration curves were linear over the concentration range of 1–500 µg/mL for both enantiomers. The results show that the method is specific, precise, and reproducible (intra‐ and interday precision relative standard deviations (RSDs) |
| doi_str_mv | 10.1002/chir.22271 |
| format | Article |
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A simple and rapid chiral high‐performance liquid chromatography (HPLC) method was developed and validated for bioanalysis of clopidogrel enantiomers on rat dried blood spots (DBS). Clopidogrel enantiomers were extracted from DBS using ethanol: methanol (80:20, v/v) and separated on a Chiralcel OJ‐H column containing cellulose tris (4‐methly benzoate) as a polysaccharide stationary phase using n‐hexane–ethanol‐diethylamine (70:30, 0.1 v/v) as a mobile phase at a flow rate of 1.0 mL/min. The detection was carried out at 220 nm using a photodiode array (PDA) detector while the elution order of the enantiomers was determined by a polarimeter connected to PDA in series. The effect of hematocrit on extraction of clopidogrel enantiomers from DBS was evaluated and no interference from endogenous substances was noticed. The overall accuracy of (R) and (S) enantiomers of clopidogrel from DBS were 91.6 and 89.2%, respectively. The calibration curves were linear over the concentration range of 1–500 µg/mL for both enantiomers. The results show that the method is specific, precise, and reproducible (intra‐ and interday precision relative standard deviations (RSDs) <10.0%). The stability of racemic clopidogrel was performed under all storage conditions and the results were found to be well within the acceptance limits. Chirality 26:102–107, 2014.© 2014 Wiley Periodicals, Inc.</description><identifier>ISSN: 0899-0042</identifier><identifier>EISSN: 1520-636X</identifier><identifier>DOI: 10.1002/chir.22271</identifier><identifier>PMID: 24436208</identifier><language>eng</language><publisher>United States: Blackwell Publishing Ltd</publisher><subject>Animals ; antiplatelets ; Biological Assay ; Blood ; Blood Chemical Analysis - methods ; cellulose tris (4-methly benzoate) on silica ; Chirality ; Chromatography, High Pressure Liquid ; clopidogrel ; DBS ; dried blood spots ; Enantiomers ; Ethyl alcohol ; hematocrit ; Methyl alcohol ; Molecular Structure ; PDA ; Rats ; Reproducibility of Results ; Spots ; Stereoisomerism ; Ticlopidine - analogs & derivatives ; Ticlopidine - analysis ; Ticlopidine - chemistry ; Time Factors</subject><ispartof>Chirality (New York, N.Y.), 2014-02, Vol.26 (2), p.102-107</ispartof><rights>Copyright © 2014 Wiley Periodicals, Inc</rights><rights>Copyright © 2014 Wiley Periodicals, Inc.</rights><rights>Copyright © 2014 John Wiley & Sons, Ltd.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c4281-ced4359b6ed45070943c3c52e355af36eb4f6e033f23c7fb6f16510d35386dd43</citedby><cites>FETCH-LOGICAL-c4281-ced4359b6ed45070943c3c52e355af36eb4f6e033f23c7fb6f16510d35386dd43</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Fchir.22271$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fchir.22271$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>314,776,780,1411,27903,27904,45553,45554</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/24436208$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Nageswara Rao, Ramisetti</creatorcontrib><creatorcontrib>Prasad, Katuri Guru</creatorcontrib><creatorcontrib>Bindu Priya, Pullakandam</creatorcontrib><creatorcontrib>Bijarji, Shriharsh</creatorcontrib><title>HPLC-PDA-ORD Bioassay of S-(+) and R-(−) Clopidogrel on Rat Dried Blood Spots</title><title>Chirality (New York, N.Y.)</title><addtitle>Chirality</addtitle><description>ABSTRACT
A simple and rapid chiral high‐performance liquid chromatography (HPLC) method was developed and validated for bioanalysis of clopidogrel enantiomers on rat dried blood spots (DBS). Clopidogrel enantiomers were extracted from DBS using ethanol: methanol (80:20, v/v) and separated on a Chiralcel OJ‐H column containing cellulose tris (4‐methly benzoate) as a polysaccharide stationary phase using n‐hexane–ethanol‐diethylamine (70:30, 0.1 v/v) as a mobile phase at a flow rate of 1.0 mL/min. The detection was carried out at 220 nm using a photodiode array (PDA) detector while the elution order of the enantiomers was determined by a polarimeter connected to PDA in series. The effect of hematocrit on extraction of clopidogrel enantiomers from DBS was evaluated and no interference from endogenous substances was noticed. The overall accuracy of (R) and (S) enantiomers of clopidogrel from DBS were 91.6 and 89.2%, respectively. The calibration curves were linear over the concentration range of 1–500 µg/mL for both enantiomers. The results show that the method is specific, precise, and reproducible (intra‐ and interday precision relative standard deviations (RSDs) <10.0%). The stability of racemic clopidogrel was performed under all storage conditions and the results were found to be well within the acceptance limits. Chirality 26:102–107, 2014.© 2014 Wiley Periodicals, Inc.</description><subject>Animals</subject><subject>antiplatelets</subject><subject>Biological Assay</subject><subject>Blood</subject><subject>Blood Chemical Analysis - methods</subject><subject>cellulose tris (4-methly benzoate) on silica</subject><subject>Chirality</subject><subject>Chromatography, High Pressure Liquid</subject><subject>clopidogrel</subject><subject>DBS</subject><subject>dried blood spots</subject><subject>Enantiomers</subject><subject>Ethyl alcohol</subject><subject>hematocrit</subject><subject>Methyl alcohol</subject><subject>Molecular Structure</subject><subject>PDA</subject><subject>Rats</subject><subject>Reproducibility of Results</subject><subject>Spots</subject><subject>Stereoisomerism</subject><subject>Ticlopidine - analogs & derivatives</subject><subject>Ticlopidine - analysis</subject><subject>Ticlopidine - chemistry</subject><subject>Time Factors</subject><issn>0899-0042</issn><issn>1520-636X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2014</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkcFOGzEURS1UBCnthg9AlroJVKbPfrZnZgmTQqARQQHU7ixnxtMOncSpnQjyB13zif2STgiwYNGu3ubcIz0dQnY5HHIA8an4UYdDIUTCN0iHKwFMo_72hnQgzTIGIMU2eRvjLQBkGuUW2RZSohaQdsiwfznI2WXviA1HPXpcexujXVJf0SvW_bhP7bSkI9b98_thn-aNn9Wl_x5cQ_2Ujuyc9kLtSnrceF_Sq5mfx3dks7JNdO-f7g65Ofl8nffZYHh6lh8NWCFFylnhSokqG-v2Kkggk1hgoYRDpWyF2o1lpR0gVgKLpBrrimvFoUSFqS7b7Q7prr2z4H8tXJybSR0L1zR26vwiGp5IqVsrx_-jCqRUQmUr64dX6K1fhGn7iOEy4xJQqKSlDtZUEXyMwVVmFuqJDUvDwayKmFUR81ikhfeelIvxxJUv6HOCFuBr4K5u3PIfKpP3z0bPUrbe1HHu7l82Nvw0OsFEma8XpwbPYZBe97-YC_wLSdyfsA</recordid><startdate>201402</startdate><enddate>201402</enddate><creator>Nageswara Rao, Ramisetti</creator><creator>Prasad, Katuri Guru</creator><creator>Bindu Priya, Pullakandam</creator><creator>Bijarji, Shriharsh</creator><general>Blackwell Publishing Ltd</general><general>Wiley Subscription Services, Inc</general><scope>BSCLL</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>7QO</scope><scope>7QR</scope><scope>7U7</scope><scope>8FD</scope><scope>C1K</scope><scope>FR3</scope><scope>P64</scope><scope>7X8</scope><scope>7SC</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>JG9</scope><scope>JQ2</scope><scope>L7M</scope><scope>L~C</scope><scope>L~D</scope></search><sort><creationdate>201402</creationdate><title>HPLC-PDA-ORD Bioassay of S-(+) and R-(−) Clopidogrel on Rat Dried Blood Spots</title><author>Nageswara Rao, Ramisetti ; Prasad, Katuri Guru ; Bindu Priya, Pullakandam ; Bijarji, Shriharsh</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c4281-ced4359b6ed45070943c3c52e355af36eb4f6e033f23c7fb6f16510d35386dd43</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2014</creationdate><topic>Animals</topic><topic>antiplatelets</topic><topic>Biological Assay</topic><topic>Blood</topic><topic>Blood Chemical Analysis - methods</topic><topic>cellulose tris (4-methly benzoate) on silica</topic><topic>Chirality</topic><topic>Chromatography, High Pressure Liquid</topic><topic>clopidogrel</topic><topic>DBS</topic><topic>dried blood spots</topic><topic>Enantiomers</topic><topic>Ethyl alcohol</topic><topic>hematocrit</topic><topic>Methyl alcohol</topic><topic>Molecular Structure</topic><topic>PDA</topic><topic>Rats</topic><topic>Reproducibility of Results</topic><topic>Spots</topic><topic>Stereoisomerism</topic><topic>Ticlopidine - analogs & derivatives</topic><topic>Ticlopidine - analysis</topic><topic>Ticlopidine - chemistry</topic><topic>Time Factors</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Nageswara Rao, Ramisetti</creatorcontrib><creatorcontrib>Prasad, Katuri Guru</creatorcontrib><creatorcontrib>Bindu Priya, Pullakandam</creatorcontrib><creatorcontrib>Bijarji, Shriharsh</creatorcontrib><collection>Istex</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Biotechnology Research Abstracts</collection><collection>Chemoreception Abstracts</collection><collection>Toxicology Abstracts</collection><collection>Technology Research Database</collection><collection>Environmental Sciences and Pollution Management</collection><collection>Engineering Research Database</collection><collection>Biotechnology and BioEngineering Abstracts</collection><collection>MEDLINE - Academic</collection><collection>Computer and Information Systems Abstracts</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Materials Research Database</collection><collection>ProQuest Computer Science Collection</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>Computer and Information Systems Abstracts Academic</collection><collection>Computer and Information Systems Abstracts Professional</collection><jtitle>Chirality (New York, N.Y.)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Nageswara Rao, Ramisetti</au><au>Prasad, Katuri Guru</au><au>Bindu Priya, Pullakandam</au><au>Bijarji, Shriharsh</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>HPLC-PDA-ORD Bioassay of S-(+) and R-(−) Clopidogrel on Rat Dried Blood Spots</atitle><jtitle>Chirality (New York, N.Y.)</jtitle><addtitle>Chirality</addtitle><date>2014-02</date><risdate>2014</risdate><volume>26</volume><issue>2</issue><spage>102</spage><epage>107</epage><pages>102-107</pages><issn>0899-0042</issn><eissn>1520-636X</eissn><abstract>ABSTRACT
A simple and rapid chiral high‐performance liquid chromatography (HPLC) method was developed and validated for bioanalysis of clopidogrel enantiomers on rat dried blood spots (DBS). Clopidogrel enantiomers were extracted from DBS using ethanol: methanol (80:20, v/v) and separated on a Chiralcel OJ‐H column containing cellulose tris (4‐methly benzoate) as a polysaccharide stationary phase using n‐hexane–ethanol‐diethylamine (70:30, 0.1 v/v) as a mobile phase at a flow rate of 1.0 mL/min. The detection was carried out at 220 nm using a photodiode array (PDA) detector while the elution order of the enantiomers was determined by a polarimeter connected to PDA in series. The effect of hematocrit on extraction of clopidogrel enantiomers from DBS was evaluated and no interference from endogenous substances was noticed. The overall accuracy of (R) and (S) enantiomers of clopidogrel from DBS were 91.6 and 89.2%, respectively. The calibration curves were linear over the concentration range of 1–500 µg/mL for both enantiomers. The results show that the method is specific, precise, and reproducible (intra‐ and interday precision relative standard deviations (RSDs) <10.0%). The stability of racemic clopidogrel was performed under all storage conditions and the results were found to be well within the acceptance limits. Chirality 26:102–107, 2014.© 2014 Wiley Periodicals, Inc.</abstract><cop>United States</cop><pub>Blackwell Publishing Ltd</pub><pmid>24436208</pmid><doi>10.1002/chir.22271</doi><tpages>6</tpages></addata></record> |
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| ispartof | Chirality (New York, N.Y.), 2014-02, Vol.26 (2), p.102-107 |
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| subjects | Animals antiplatelets Biological Assay Blood Blood Chemical Analysis - methods cellulose tris (4-methly benzoate) on silica Chirality Chromatography, High Pressure Liquid clopidogrel DBS dried blood spots Enantiomers Ethyl alcohol hematocrit Methyl alcohol Molecular Structure PDA Rats Reproducibility of Results Spots Stereoisomerism Ticlopidine - analogs & derivatives Ticlopidine - analysis Ticlopidine - chemistry Time Factors |
| title | HPLC-PDA-ORD Bioassay of S-(+) and R-(−) Clopidogrel on Rat Dried Blood Spots |
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