Determination of plasma Vitamin K by high-performance liquid chromatography with fluorescence detection using Vitamin K analogs as internal standards
A HPLC fluorescence determination method for Vitamin K derivatives (Vitamin K 1, phylloquinone, PK and K 2, menaquinones, MK-4 and MK-7) using post-column reduction and internal standards was developed. Selectivity and reproducibility were increased by optimized chromatography conditions and satisfa...
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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, 2005-02, Vol.816 (1), p.41-48 |
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container_title | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences |
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creator | Kamao, Maya Suhara, Yoshitomo Tsugawa, Naoko Okano, Toshio |
description | A HPLC fluorescence determination method for Vitamin K derivatives (Vitamin K
1, phylloquinone, PK and K
2, menaquinones, MK-4 and MK-7) using post-column reduction and internal standards was developed. Selectivity and reproducibility were increased by optimized chromatography conditions and satisfactory precision and accuracy were attained by using synthetic internal standards. After addition of internal standards to plasma samples, lipids were extracted with ethanol and hexane. Chromatography was performed by isocratic reverse phase separation on a C18 column. Vitamin K derivatives were detected at 430
nm with excitation at 320
nm for MK-4 and 240
nm for PK and MK-7. The detection limits for MK-4, PK and MK-7 were 4, 2 and 4
pg, respectively. The recoveries of MK-4, PK and MK-7 were greater than 92% and the inter- and intra-assay R.S.D. values were 5.7–9.2% for MK-4, 4.9–9.6% for PK and 6.3–19.3% for MK-7. The data showed good correlation between proposed method and LC-APCI/MS method for MK-4 (
R
2
=
0.988), PK (
R
2
=
0.979) and MK-7 (
R
2
=
0.986). The method allows the determination of Vitamin K for evaluating their clinical and nutritional status. |
doi_str_mv | 10.1016/j.jchromb.2004.11.003 |
format | Article |
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1, phylloquinone, PK and K
2, menaquinones, MK-4 and MK-7) using post-column reduction and internal standards was developed. Selectivity and reproducibility were increased by optimized chromatography conditions and satisfactory precision and accuracy were attained by using synthetic internal standards. After addition of internal standards to plasma samples, lipids were extracted with ethanol and hexane. Chromatography was performed by isocratic reverse phase separation on a C18 column. Vitamin K derivatives were detected at 430
nm with excitation at 320
nm for MK-4 and 240
nm for PK and MK-7. The detection limits for MK-4, PK and MK-7 were 4, 2 and 4
pg, respectively. The recoveries of MK-4, PK and MK-7 were greater than 92% and the inter- and intra-assay R.S.D. values were 5.7–9.2% for MK-4, 4.9–9.6% for PK and 6.3–19.3% for MK-7. The data showed good correlation between proposed method and LC-APCI/MS method for MK-4 (
R
2
=
0.988), PK (
R
2
=
0.979) and MK-7 (
R
2
=
0.986). The method allows the determination of Vitamin K for evaluating their clinical and nutritional status.</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2004.11.003</identifier><identifier>PMID: 15664332</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical, structural and metabolic biochemistry ; Biological and medical sciences ; Chromatography, High Pressure Liquid - methods ; Fluorescence ; Fluorescence detection ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; Humans ; Internal standards ; Medical sciences ; Osteoporosis - blood ; Osteoporosis - drug therapy ; Pharmacology. Drug treatments ; Reference Standards ; Spectrometry, Mass, Electrospray Ionization ; Vitamin K ; Vitamin K - analogs & derivatives ; Vitamin K - blood ; Vitamin K 2 - analogs & derivatives ; Vitamin K 2 - blood ; Vitamin K 2 - therapeutic use</subject><ispartof>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2005-02, Vol.816 (1), p.41-48</ispartof><rights>2004 Elsevier B.V.</rights><rights>2005 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c422t-d3aaef49375c9e72fc87d02dc0cd4da6a7bddee66676d6bbf791e3c998e710983</citedby><cites>FETCH-LOGICAL-c422t-d3aaef49375c9e72fc87d02dc0cd4da6a7bddee66676d6bbf791e3c998e710983</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.2004.11.003$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=16451357$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/15664332$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Kamao, Maya</creatorcontrib><creatorcontrib>Suhara, Yoshitomo</creatorcontrib><creatorcontrib>Tsugawa, Naoko</creatorcontrib><creatorcontrib>Okano, Toshio</creatorcontrib><title>Determination of plasma Vitamin K by high-performance liquid chromatography with fluorescence detection using Vitamin K analogs as internal standards</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 HPLC fluorescence determination method for Vitamin K derivatives (Vitamin K
1, phylloquinone, PK and K
2, menaquinones, MK-4 and MK-7) using post-column reduction and internal standards was developed. Selectivity and reproducibility were increased by optimized chromatography conditions and satisfactory precision and accuracy were attained by using synthetic internal standards. After addition of internal standards to plasma samples, lipids were extracted with ethanol and hexane. Chromatography was performed by isocratic reverse phase separation on a C18 column. Vitamin K derivatives were detected at 430
nm with excitation at 320
nm for MK-4 and 240
nm for PK and MK-7. The detection limits for MK-4, PK and MK-7 were 4, 2 and 4
pg, respectively. The recoveries of MK-4, PK and MK-7 were greater than 92% and the inter- and intra-assay R.S.D. values were 5.7–9.2% for MK-4, 4.9–9.6% for PK and 6.3–19.3% for MK-7. The data showed good correlation between proposed method and LC-APCI/MS method for MK-4 (
R
2
=
0.988), PK (
R
2
=
0.979) and MK-7 (
R
2
=
0.986). The method allows the determination of Vitamin K for evaluating their clinical and nutritional status.</description><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Biological and medical sciences</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Fluorescence</subject><subject>Fluorescence detection</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>Humans</subject><subject>Internal standards</subject><subject>Medical sciences</subject><subject>Osteoporosis - blood</subject><subject>Osteoporosis - drug therapy</subject><subject>Pharmacology. Drug treatments</subject><subject>Reference Standards</subject><subject>Spectrometry, Mass, Electrospray Ionization</subject><subject>Vitamin K</subject><subject>Vitamin K - analogs & derivatives</subject><subject>Vitamin K - blood</subject><subject>Vitamin K 2 - analogs & derivatives</subject><subject>Vitamin K 2 - blood</subject><subject>Vitamin K 2 - therapeutic use</subject><issn>1570-0232</issn><issn>1873-376X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2005</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkc2O1DAQhC0EYpeFRwD5ArcEO07syQmh5VesxAUQN6tjtyceJXHWTkDzILwvnp1Iy42Tf_R1damKkOeclZxx-fpQHkwfw9iVFWN1yXnJmHhALvlOiUIo-fNhvjeKFawS1QV5ktKBMa6YEo_JBW-krIWoLsmfd7hgHP0Eiw8TDY7OA6QR6A-_QP6mX2h3pL3f98WM0YU4wmSQDv529ZbeOYAl7CPM_ZH-9ktP3bCGiMngibNZ3dwpr8lP-39UYYIh7BOFRP2ULeQnTQtMFqJNT8kjB0PCZ9t5Rb5_eP_t-lNx8_Xj5-u3N4Wpq2oprABAV7dCNaZFVTmzU5ZV1jBjawsSVGctopRSSSu7zqmWozBtu0PFWbsTV-TVWXeO4XbFtOjRZ-fDABOGNWmphKoEazPYnEETQ0oRnZ6jHyEeNWf61Ic-6K0PfepDc65zH3nuxbZg7Ua091NbARl4uQGQDAwu5nh9uudk3XDRqMy9OXOY4_jlMepk_Cli62NOWNvg_2PlLxt3sF0</recordid><startdate>20050225</startdate><enddate>20050225</enddate><creator>Kamao, Maya</creator><creator>Suhara, Yoshitomo</creator><creator>Tsugawa, Naoko</creator><creator>Okano, Toshio</creator><general>Elsevier B.V</general><general>Elsevier Science</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>20050225</creationdate><title>Determination of plasma Vitamin K by high-performance liquid chromatography with fluorescence detection using Vitamin K analogs as internal standards</title><author>Kamao, Maya ; Suhara, Yoshitomo ; Tsugawa, Naoko ; Okano, Toshio</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c422t-d3aaef49375c9e72fc87d02dc0cd4da6a7bddee66676d6bbf791e3c998e710983</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2005</creationdate><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Biological and medical sciences</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Fluorescence</topic><topic>Fluorescence detection</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>Humans</topic><topic>Internal standards</topic><topic>Medical sciences</topic><topic>Osteoporosis - blood</topic><topic>Osteoporosis - drug therapy</topic><topic>Pharmacology. Drug treatments</topic><topic>Reference Standards</topic><topic>Spectrometry, Mass, Electrospray Ionization</topic><topic>Vitamin K</topic><topic>Vitamin K - analogs & derivatives</topic><topic>Vitamin K - blood</topic><topic>Vitamin K 2 - analogs & derivatives</topic><topic>Vitamin K 2 - blood</topic><topic>Vitamin K 2 - therapeutic use</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Kamao, Maya</creatorcontrib><creatorcontrib>Suhara, Yoshitomo</creatorcontrib><creatorcontrib>Tsugawa, Naoko</creatorcontrib><creatorcontrib>Okano, Toshio</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>Kamao, Maya</au><au>Suhara, Yoshitomo</au><au>Tsugawa, Naoko</au><au>Okano, Toshio</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of plasma Vitamin K by high-performance liquid chromatography with fluorescence detection using Vitamin K analogs as internal standards</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>2005-02-25</date><risdate>2005</risdate><volume>816</volume><issue>1</issue><spage>41</spage><epage>48</epage><pages>41-48</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>A HPLC fluorescence determination method for Vitamin K derivatives (Vitamin K
1, phylloquinone, PK and K
2, menaquinones, MK-4 and MK-7) using post-column reduction and internal standards was developed. Selectivity and reproducibility were increased by optimized chromatography conditions and satisfactory precision and accuracy were attained by using synthetic internal standards. After addition of internal standards to plasma samples, lipids were extracted with ethanol and hexane. Chromatography was performed by isocratic reverse phase separation on a C18 column. Vitamin K derivatives were detected at 430
nm with excitation at 320
nm for MK-4 and 240
nm for PK and MK-7. The detection limits for MK-4, PK and MK-7 were 4, 2 and 4
pg, respectively. The recoveries of MK-4, PK and MK-7 were greater than 92% and the inter- and intra-assay R.S.D. values were 5.7–9.2% for MK-4, 4.9–9.6% for PK and 6.3–19.3% for MK-7. The data showed good correlation between proposed method and LC-APCI/MS method for MK-4 (
R
2
=
0.988), PK (
R
2
=
0.979) and MK-7 (
R
2
=
0.986). The method allows the determination of Vitamin K for evaluating their clinical and nutritional status.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>15664332</pmid><doi>10.1016/j.jchromb.2004.11.003</doi><tpages>8</tpages></addata></record> |
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language | eng |
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source | MEDLINE; Elsevier ScienceDirect Journals Complete |
subjects | Analysis Analytical, structural and metabolic biochemistry Biological and medical sciences Chromatography, High Pressure Liquid - methods Fluorescence Fluorescence detection Fundamental and applied biological sciences. Psychology General pharmacology Humans Internal standards Medical sciences Osteoporosis - blood Osteoporosis - drug therapy Pharmacology. Drug treatments Reference Standards Spectrometry, Mass, Electrospray Ionization Vitamin K Vitamin K - analogs & derivatives Vitamin K - blood Vitamin K 2 - analogs & derivatives Vitamin K 2 - blood Vitamin K 2 - therapeutic use |
title | Determination of plasma Vitamin K by high-performance liquid chromatography with fluorescence detection using Vitamin K analogs as internal standards |
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