Determination of naftopidil enantiomers in rat plasma using chiral solid phases and pre-column derivatization high-performance liquid chromatography

► We developed two chiral RP-HPLC methods to quantify naftopidil enantiomers in plasma. ► Both of the methods were validated and met the demands of bioanalysis. ► The CSPs method was more suitable for pharmacokinetics study of (+)- and (−)-NAF. ► We determined (+)- and (−)-NAF after intravenous inje...

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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, 2012-10, Vol.907, p.140-145
Hauptverfasser: Liu, Xiawen, Zhang, Yunying, Yuan, Mu, Sun, Yinxiang
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Zhang, Yunying
Yuan, Mu
Sun, Yinxiang
description ► We developed two chiral RP-HPLC methods to quantify naftopidil enantiomers in plasma. ► Both of the methods were validated and met the demands of bioanalysis. ► The CSPs method was more suitable for pharmacokinetics study of (+)- and (−)-NAF. ► We determined (+)- and (−)-NAF after intravenous injection of (±)-NAF by CSPs HPLC. Two bioanalytical HPLC methods (chiral solid phases (CSPs) HPLC and pre-column derivatization HPLC) were developed and validated for the determination of naftopidil enantiomers in rat plasma. Analytes were extracted from biomaterials by liquid–liquid extraction. The pre-column derivatization HPLC method employed (+)-diacetyl-l-tartaric anhydride (DATAN) as the pre-column derivatization reagent, and subsequent separation of diastereomers was conducted on an Agilent Hypersil ODS column with a mixture of methanol–acetonitrile–phosphate buffer (pH 4.1; 20mM) (40:30:30, v/v/v) flowing at 1mL/min as the mobile phase. The CSPs HPLC method utilized a Chiralpak IA column with a mobile phase of methanol–acetonitrile–acetate buffer (pH 5.3; 5mM) (50:25:25, v/v/v) flowing at 0.5mL/min. In both methods, the analytes were monitored using a fluorescence detector with an excitation wavelength of 290nm and an emission wavelength of 340nm. Both methods were consistent (RSD
doi_str_mv 10.1016/j.jchromb.2012.09.021
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Two bioanalytical HPLC methods (chiral solid phases (CSPs) HPLC and pre-column derivatization HPLC) were developed and validated for the determination of naftopidil enantiomers in rat plasma. Analytes were extracted from biomaterials by liquid–liquid extraction. The pre-column derivatization HPLC method employed (+)-diacetyl-l-tartaric anhydride (DATAN) as the pre-column derivatization reagent, and subsequent separation of diastereomers was conducted on an Agilent Hypersil ODS column with a mixture of methanol–acetonitrile–phosphate buffer (pH 4.1; 20mM) (40:30:30, v/v/v) flowing at 1mL/min as the mobile phase. The CSPs HPLC method utilized a Chiralpak IA column with a mobile phase of methanol–acetonitrile–acetate buffer (pH 5.3; 5mM) (50:25:25, v/v/v) flowing at 0.5mL/min. In both methods, the analytes were monitored using a fluorescence detector with an excitation wavelength of 290nm and an emission wavelength of 340nm. Both methods were consistent (RSD&lt;15% by the derivatization method and&lt;10% by the CSPs method) and linear (r&gt;9950). Compared to the pre-column derivatization method, the CSPs method had lower quantification limits (10.6/9.6ng/mL of (+)-/(−)-naftopidil by derivatization method and 1.1/1.8ng/mL of (+)-/(−)-naftopidil by CSPs method), and was simpler to carry out. The validated CSPs method was successfully applied in a pharmacokinetic study of naftopidil enantiomers in rats, which showed that pharmacokinetic parameters of (+)- and (−)-NAF after intravenous administration of (±)-NAF were similar.</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2012.09.021</identifier><identifier>PMID: 23026227</identifier><language>eng</language><publisher>Netherlands: Elsevier B.V</publisher><subject>Anhydrides ; Animals ; biocompatible materials ; Buffers ; Chiral column ; Chromatography, High Pressure Liquid - methods ; derivatization ; Detectors ; diastereomers ; Drug Stability ; Enantiomers ; Enantioselective pharmacokinetics ; Female ; fluorescence ; high performance liquid chromatography ; intravenous injection ; Linear Models ; Liquid chromatography ; Liquid-Liquid Extraction ; Male ; Naftopidil ; Naphthalenes - blood ; Naphthalenes - chemistry ; Naphthalenes - pharmacokinetics ; pharmacokinetics ; Piperazines - blood ; Piperazines - chemistry ; Piperazines - pharmacokinetics ; Pre-column derivatization ; Rats ; Rats, Sprague-Dawley ; Reproducibility of Results ; Sensitivity and Specificity ; Solid phases ; Stereoisomerism ; Wavelengths</subject><ispartof>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2012-10, Vol.907, p.140-145</ispartof><rights>2012 Elsevier B.V.</rights><rights>Copyright © 2012 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c422t-c901b19e09fc288d68620c00141b705c122750aa8fbfe693fbfb5302510e6fc83</citedby><cites>FETCH-LOGICAL-c422t-c901b19e09fc288d68620c00141b705c122750aa8fbfe693fbfb5302510e6fc83</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.jchromb.2012.09.021$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3548,27923,27924,45994</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/23026227$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Liu, Xiawen</creatorcontrib><creatorcontrib>Zhang, Yunying</creatorcontrib><creatorcontrib>Yuan, Mu</creatorcontrib><creatorcontrib>Sun, Yinxiang</creatorcontrib><title>Determination of naftopidil enantiomers in rat plasma using chiral solid phases and pre-column derivatization high-performance liquid chromatography</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>► We developed two chiral RP-HPLC methods to quantify naftopidil enantiomers in plasma. ► Both of the methods were validated and met the demands of bioanalysis. ► The CSPs method was more suitable for pharmacokinetics study of (+)- and (−)-NAF. ► We determined (+)- and (−)-NAF after intravenous injection of (±)-NAF by CSPs HPLC. Two bioanalytical HPLC methods (chiral solid phases (CSPs) HPLC and pre-column derivatization HPLC) were developed and validated for the determination of naftopidil enantiomers in rat plasma. Analytes were extracted from biomaterials by liquid–liquid extraction. The pre-column derivatization HPLC method employed (+)-diacetyl-l-tartaric anhydride (DATAN) as the pre-column derivatization reagent, and subsequent separation of diastereomers was conducted on an Agilent Hypersil ODS column with a mixture of methanol–acetonitrile–phosphate buffer (pH 4.1; 20mM) (40:30:30, v/v/v) flowing at 1mL/min as the mobile phase. The CSPs HPLC method utilized a Chiralpak IA column with a mobile phase of methanol–acetonitrile–acetate buffer (pH 5.3; 5mM) (50:25:25, v/v/v) flowing at 0.5mL/min. In both methods, the analytes were monitored using a fluorescence detector with an excitation wavelength of 290nm and an emission wavelength of 340nm. Both methods were consistent (RSD&lt;15% by the derivatization method and&lt;10% by the CSPs method) and linear (r&gt;9950). Compared to the pre-column derivatization method, the CSPs method had lower quantification limits (10.6/9.6ng/mL of (+)-/(−)-naftopidil by derivatization method and 1.1/1.8ng/mL of (+)-/(−)-naftopidil by CSPs method), and was simpler to carry out. The validated CSPs method was successfully applied in a pharmacokinetic study of naftopidil enantiomers in rats, which showed that pharmacokinetic parameters of (+)- and (−)-NAF after intravenous administration of (±)-NAF were similar.</description><subject>Anhydrides</subject><subject>Animals</subject><subject>biocompatible materials</subject><subject>Buffers</subject><subject>Chiral column</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>derivatization</subject><subject>Detectors</subject><subject>diastereomers</subject><subject>Drug Stability</subject><subject>Enantiomers</subject><subject>Enantioselective pharmacokinetics</subject><subject>Female</subject><subject>fluorescence</subject><subject>high performance liquid chromatography</subject><subject>intravenous injection</subject><subject>Linear Models</subject><subject>Liquid chromatography</subject><subject>Liquid-Liquid Extraction</subject><subject>Male</subject><subject>Naftopidil</subject><subject>Naphthalenes - blood</subject><subject>Naphthalenes - chemistry</subject><subject>Naphthalenes - pharmacokinetics</subject><subject>pharmacokinetics</subject><subject>Piperazines - blood</subject><subject>Piperazines - chemistry</subject><subject>Piperazines - pharmacokinetics</subject><subject>Pre-column derivatization</subject><subject>Rats</subject><subject>Rats, Sprague-Dawley</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Solid phases</subject><subject>Stereoisomerism</subject><subject>Wavelengths</subject><issn>1570-0232</issn><issn>1873-376X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkc1u1TAQhSMEoj_wCICXbBLGTmInK4RaaJEqsYBK7CzHGd_4KrFTO6nUPkcfGLe5dNvVjKxvzvjMybIPFAoKlH_ZF3s9BD91BQPKCmgLYPRVdkwbUeal4H9fp74WkAMr2VF2EuMegAoQ5dvsiJXAOGPiOHs4xwXDZJ1arHfEG-KUWfxsezsSdMql5wlDJNaRoBYyjypOiqzRuh3Rgw1qJNGPtifzoCJGolxqA-baj-vkSI_B3ibt-01_sLshnzEYHyblNJLR3qxp-MmKWvwuqHm4e5e9MWqM-P5QT7PrH9__nF3mV78ufp59u8p1xdiS6xZoR1uE1mjWND1vOAOdXFa0E1BrmhzWoFRjOoO8LVPp6uS8poDc6KY8zT5vunPwNyvGRU42ahxH5dCvUSYB2nAhGH0ZpZSVVQlVldB6Q3XwMQY0cg52UuFOUpCP2cm9PGQnH7OT0Ep4WvHxsGLtJuyfp_6HlYBPG2CUl2oXbJTXv5MCBwAuOK0T8XUjMF3t1mKQUVtMd-5tQL3I3tsXPvEPyeC5pg</recordid><startdate>20121015</startdate><enddate>20121015</enddate><creator>Liu, Xiawen</creator><creator>Zhang, Yunying</creator><creator>Yuan, Mu</creator><creator>Sun, Yinxiang</creator><general>Elsevier B.V</general><scope>FBQ</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><scope>7TB</scope><scope>8FD</scope><scope>FR3</scope></search><sort><creationdate>20121015</creationdate><title>Determination of naftopidil enantiomers in rat plasma using chiral solid phases and pre-column derivatization high-performance liquid chromatography</title><author>Liu, Xiawen ; Zhang, Yunying ; Yuan, Mu ; Sun, Yinxiang</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c422t-c901b19e09fc288d68620c00141b705c122750aa8fbfe693fbfb5302510e6fc83</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2012</creationdate><topic>Anhydrides</topic><topic>Animals</topic><topic>biocompatible materials</topic><topic>Buffers</topic><topic>Chiral column</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>derivatization</topic><topic>Detectors</topic><topic>diastereomers</topic><topic>Drug Stability</topic><topic>Enantiomers</topic><topic>Enantioselective pharmacokinetics</topic><topic>Female</topic><topic>fluorescence</topic><topic>high performance liquid chromatography</topic><topic>intravenous injection</topic><topic>Linear Models</topic><topic>Liquid chromatography</topic><topic>Liquid-Liquid Extraction</topic><topic>Male</topic><topic>Naftopidil</topic><topic>Naphthalenes - blood</topic><topic>Naphthalenes - chemistry</topic><topic>Naphthalenes - pharmacokinetics</topic><topic>pharmacokinetics</topic><topic>Piperazines - blood</topic><topic>Piperazines - chemistry</topic><topic>Piperazines - pharmacokinetics</topic><topic>Pre-column derivatization</topic><topic>Rats</topic><topic>Rats, Sprague-Dawley</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Solid phases</topic><topic>Stereoisomerism</topic><topic>Wavelengths</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Liu, Xiawen</creatorcontrib><creatorcontrib>Zhang, Yunying</creatorcontrib><creatorcontrib>Yuan, Mu</creatorcontrib><creatorcontrib>Sun, Yinxiang</creatorcontrib><collection>AGRIS</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><collection>Mechanical &amp; 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B, Analytical technologies in the biomedical and life sciences</jtitle><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><date>2012-10-15</date><risdate>2012</risdate><volume>907</volume><spage>140</spage><epage>145</epage><pages>140-145</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>► We developed two chiral RP-HPLC methods to quantify naftopidil enantiomers in plasma. ► Both of the methods were validated and met the demands of bioanalysis. ► The CSPs method was more suitable for pharmacokinetics study of (+)- and (−)-NAF. ► We determined (+)- and (−)-NAF after intravenous injection of (±)-NAF by CSPs HPLC. Two bioanalytical HPLC methods (chiral solid phases (CSPs) HPLC and pre-column derivatization HPLC) were developed and validated for the determination of naftopidil enantiomers in rat plasma. Analytes were extracted from biomaterials by liquid–liquid extraction. The pre-column derivatization HPLC method employed (+)-diacetyl-l-tartaric anhydride (DATAN) as the pre-column derivatization reagent, and subsequent separation of diastereomers was conducted on an Agilent Hypersil ODS column with a mixture of methanol–acetonitrile–phosphate buffer (pH 4.1; 20mM) (40:30:30, v/v/v) flowing at 1mL/min as the mobile phase. The CSPs HPLC method utilized a Chiralpak IA column with a mobile phase of methanol–acetonitrile–acetate buffer (pH 5.3; 5mM) (50:25:25, v/v/v) flowing at 0.5mL/min. In both methods, the analytes were monitored using a fluorescence detector with an excitation wavelength of 290nm and an emission wavelength of 340nm. Both methods were consistent (RSD&lt;15% by the derivatization method and&lt;10% by the CSPs method) and linear (r&gt;9950). Compared to the pre-column derivatization method, the CSPs method had lower quantification limits (10.6/9.6ng/mL of (+)-/(−)-naftopidil by derivatization method and 1.1/1.8ng/mL of (+)-/(−)-naftopidil by CSPs method), and was simpler to carry out. The validated CSPs method was successfully applied in a pharmacokinetic study of naftopidil enantiomers in rats, which showed that pharmacokinetic parameters of (+)- and (−)-NAF after intravenous administration of (±)-NAF were similar.</abstract><cop>Netherlands</cop><pub>Elsevier B.V</pub><pmid>23026227</pmid><doi>10.1016/j.jchromb.2012.09.021</doi><tpages>6</tpages></addata></record>
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subjects Anhydrides
Animals
biocompatible materials
Buffers
Chiral column
Chromatography, High Pressure Liquid - methods
derivatization
Detectors
diastereomers
Drug Stability
Enantiomers
Enantioselective pharmacokinetics
Female
fluorescence
high performance liquid chromatography
intravenous injection
Linear Models
Liquid chromatography
Liquid-Liquid Extraction
Male
Naftopidil
Naphthalenes - blood
Naphthalenes - chemistry
Naphthalenes - pharmacokinetics
pharmacokinetics
Piperazines - blood
Piperazines - chemistry
Piperazines - pharmacokinetics
Pre-column derivatization
Rats
Rats, Sprague-Dawley
Reproducibility of Results
Sensitivity and Specificity
Solid phases
Stereoisomerism
Wavelengths
title Determination of naftopidil enantiomers in rat plasma using chiral solid phases and pre-column derivatization high-performance liquid chromatography
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