Quantitative determination of glycopyrrolate in human plasma by liquid chromatography–electrospray ionization mass spectrometry: The use of a volatile ion-pairing agent during both liquid–liquid extraction and liquid chromatography
The work presented here deals with the development of a quantitative tool for the determination of the quaternary ammonium anticholinergic glycopyrrolate in human plasma samples. Mepenzolate was used as an internal standard. The plasma samples were subjected to a suitable sample clean-up consisting...
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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.24-30 |
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container_title | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences |
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creator | Storme, M.L. t’Kindt, R.S. Goeteyn, W. Reyntjens, K. Van Bocxlaer, J.F. |
description | The work presented here deals with the development of a quantitative tool for the determination of the quaternary ammonium anticholinergic glycopyrrolate in human plasma samples. Mepenzolate was used as an internal standard. The plasma samples were subjected to a suitable sample clean-up consisting of a simple and relatively fast, two step liquid–liquid ion-pair extraction procedure. The chromatography, using the same volatile ion-pair reagent heptafluorobutyric acid (HFBA), takes only 10
min. Relative standard deviation of retention times was never above 2.26% (
n
=
36). The method was fully validated based on the US FDA Bioanalytical Method Validation Guidance for Industry. As such, a quantitative ESI-LC–MS(/MS) (TOF mass spectrometry) method was optimized for the absolute quantification of glycopyrrolate in human plasma in a concentration range from 0.101 to 101
ng/mL using a quadratic calibration function (
R
2
=
0.9995),
y
=
−2.21
×
10
−4 (±3.93
×
10
−5)
×
x
2
+
5.85
×
10
−2 (±5.27
×
10
−3)
×
x
+
4.08
×
10
−3 (±4.82
×
10
−4). For the three QC concentrations (QC
1 0.252, QC
2 2.52, and QC
3 25.2
ng/mL) and the LLOQ (0.101
ng/mL), total precision was under 20% (18.0% (
n
=
6) at the LLOQ) and maximum accuracy was 112% (88.9% for the LLOQ,
n
=
6). Absolute matrix effect (maximum 133%
±
9.59,
n
=
3), absolute recovery (better than 41.8%
±
2.22,
n
=
3), relative (inter-subject) matrix effect (maximum 10.9%
±
1.45,
n
=
4) and process efficiency (better than 45.2%
±
5.74,
n
=
3) too were assessed at the 3 QC concentrations. |
doi_str_mv | 10.1016/j.jchromb.2008.10.013 |
format | Article |
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min. Relative standard deviation of retention times was never above 2.26% (
n
=
36). The method was fully validated based on the US FDA Bioanalytical Method Validation Guidance for Industry. As such, a quantitative ESI-LC–MS(/MS) (TOF mass spectrometry) method was optimized for the absolute quantification of glycopyrrolate in human plasma in a concentration range from 0.101 to 101
ng/mL using a quadratic calibration function (
R
2
=
0.9995),
y
=
−2.21
×
10
−4 (±3.93
×
10
−5)
×
x
2
+
5.85
×
10
−2 (±5.27
×
10
−3)
×
x
+
4.08
×
10
−3 (±4.82
×
10
−4). For the three QC concentrations (QC
1 0.252, QC
2 2.52, and QC
3 25.2
ng/mL) and the LLOQ (0.101
ng/mL), total precision was under 20% (18.0% (
n
=
6) at the LLOQ) and maximum accuracy was 112% (88.9% for the LLOQ,
n
=
6). Absolute matrix effect (maximum 133%
±
9.59,
n
=
3), absolute recovery (better than 41.8%
±
2.22,
n
=
3), relative (inter-subject) matrix effect (maximum 10.9%
±
1.45,
n
=
4) and process efficiency (better than 45.2%
±
5.74,
n
=
3) too were assessed at the 3 QC concentrations.</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2008.10.013</identifier><identifier>PMID: 18977186</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical, structural and metabolic biochemistry ; Biological and medical sciences ; Chemical Fractionation - methods ; Chromatography, High Pressure Liquid - methods ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; Glycopyrrolate ; Glycopyrrolate - blood ; Humans ; LC–MS/MS ; Medical sciences ; Pharmacokinetics ; Pharmacology. Drug treatments ; Reproducibility of Results ; Spectrometry, Mass, Electrospray Ionization - methods ; Tandem Mass Spectrometry - methods</subject><ispartof>Journal of chromatography. B, Analytical technologies in the biomedical and life sciences, 2008-12, Vol.876 (1), p.24-30</ispartof><rights>2008 Elsevier B.V.</rights><rights>2009 INIST-CNRS</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c469t-a475f7caa3e4eb9aa7469af49b8e63e0e6a22d0033b707f20b8ff9641bdd7bbc3</citedby><cites>FETCH-LOGICAL-c469t-a475f7caa3e4eb9aa7469af49b8e63e0e6a22d0033b707f20b8ff9641bdd7bbc3</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.2008.10.013$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=20951749$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/18977186$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Storme, M.L.</creatorcontrib><creatorcontrib>t’Kindt, R.S.</creatorcontrib><creatorcontrib>Goeteyn, W.</creatorcontrib><creatorcontrib>Reyntjens, K.</creatorcontrib><creatorcontrib>Van Bocxlaer, J.F.</creatorcontrib><title>Quantitative determination of glycopyrrolate in human plasma by liquid chromatography–electrospray ionization mass spectrometry: The use of a volatile ion-pairing agent during both liquid–liquid extraction and 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>The work presented here deals with the development of a quantitative tool for the determination of the quaternary ammonium anticholinergic glycopyrrolate in human plasma samples. Mepenzolate was used as an internal standard. The plasma samples were subjected to a suitable sample clean-up consisting of a simple and relatively fast, two step liquid–liquid ion-pair extraction procedure. The chromatography, using the same volatile ion-pair reagent heptafluorobutyric acid (HFBA), takes only 10
min. Relative standard deviation of retention times was never above 2.26% (
n
=
36). The method was fully validated based on the US FDA Bioanalytical Method Validation Guidance for Industry. As such, a quantitative ESI-LC–MS(/MS) (TOF mass spectrometry) method was optimized for the absolute quantification of glycopyrrolate in human plasma in a concentration range from 0.101 to 101
ng/mL using a quadratic calibration function (
R
2
=
0.9995),
y
=
−2.21
×
10
−4 (±3.93
×
10
−5)
×
x
2
+
5.85
×
10
−2 (±5.27
×
10
−3)
×
x
+
4.08
×
10
−3 (±4.82
×
10
−4). For the three QC concentrations (QC
1 0.252, QC
2 2.52, and QC
3 25.2
ng/mL) and the LLOQ (0.101
ng/mL), total precision was under 20% (18.0% (
n
=
6) at the LLOQ) and maximum accuracy was 112% (88.9% for the LLOQ,
n
=
6). Absolute matrix effect (maximum 133%
±
9.59,
n
=
3), absolute recovery (better than 41.8%
±
2.22,
n
=
3), relative (inter-subject) matrix effect (maximum 10.9%
±
1.45,
n
=
4) and process efficiency (better than 45.2%
±
5.74,
n
=
3) too were assessed at the 3 QC concentrations.</description><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Biological and medical sciences</subject><subject>Chemical Fractionation - methods</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>Glycopyrrolate</subject><subject>Glycopyrrolate - blood</subject><subject>Humans</subject><subject>LC–MS/MS</subject><subject>Medical sciences</subject><subject>Pharmacokinetics</subject><subject>Pharmacology. Drug treatments</subject><subject>Reproducibility of Results</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Tandem Mass Spectrometry - methods</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>eNqFkc9u1DAQxiMEoqXwCCBf4JbFTrJxwgVVFf-kSgipSNyisTPZeOXYqe2sCKe-Q9-QKy-BsxvBBYmTPTO_mW80X5I8Z3TDKCtf7zd72Ts7iE1GaRVzG8ryB8k5q3ie5rz89jD-t5ymNMuzs-SJ93tKGac8f5ycsarmnFXlefLrywQmqABBHZC0GNANysTIGmI7stOztOPsnNUQkChD-mkAQ0YNfgAiZqLV7aRactwFgt05GPv55909apTBWT86mEmcpn6chg7gPfHjsThgcPMbctMjmTwuekAOi5LSuPSkIyinzI7ADk0g7XQMhA39Kht1Vn38HhzIowKY9t9bPU0edaA9Plvfi-Tr-3c3Vx_T688fPl1dXqeyKOuQQsG3HZcAORYoagAe09AVtaiwzJFiCVnWUprnIp6zy6iouq4uCybalgsh84vk1Wnu6OzthD40g_IStQaDdvJNWVdZWdEygtsTKOOhvMOuGZ0awM0No83icrNvVpebxeUlHV2OfS9WgUkM2P7tWm2NwMsVAC9Bdw6MVP4Pl9F6y3hRR-7ticN4joNC13ip0EhslYsONa1V_1nlN0Z21MY</recordid><startdate>20081201</startdate><enddate>20081201</enddate><creator>Storme, M.L.</creator><creator>t’Kindt, R.S.</creator><creator>Goeteyn, W.</creator><creator>Reyntjens, K.</creator><creator>Van Bocxlaer, J.F.</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>Quantitative determination of glycopyrrolate in human plasma by liquid chromatography–electrospray ionization mass spectrometry: The use of a volatile ion-pairing agent during both liquid–liquid extraction and liquid chromatography</title><author>Storme, M.L. ; t’Kindt, R.S. ; Goeteyn, W. ; Reyntjens, K. ; Van Bocxlaer, J.F.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c469t-a475f7caa3e4eb9aa7469af49b8e63e0e6a22d0033b707f20b8ff9641bdd7bbc3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2008</creationdate><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Biological and medical sciences</topic><topic>Chemical Fractionation - methods</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>Glycopyrrolate</topic><topic>Glycopyrrolate - blood</topic><topic>Humans</topic><topic>LC–MS/MS</topic><topic>Medical sciences</topic><topic>Pharmacokinetics</topic><topic>Pharmacology. Drug treatments</topic><topic>Reproducibility of Results</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Tandem Mass Spectrometry - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Storme, M.L.</creatorcontrib><creatorcontrib>t’Kindt, R.S.</creatorcontrib><creatorcontrib>Goeteyn, W.</creatorcontrib><creatorcontrib>Reyntjens, K.</creatorcontrib><creatorcontrib>Van Bocxlaer, J.F.</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>Storme, M.L.</au><au>t’Kindt, R.S.</au><au>Goeteyn, W.</au><au>Reyntjens, K.</au><au>Van Bocxlaer, J.F.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Quantitative determination of glycopyrrolate in human plasma by liquid chromatography–electrospray ionization mass spectrometry: The use of a volatile ion-pairing agent during both liquid–liquid extraction and liquid chromatography</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>24</spage><epage>30</epage><pages>24-30</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>The work presented here deals with the development of a quantitative tool for the determination of the quaternary ammonium anticholinergic glycopyrrolate in human plasma samples. Mepenzolate was used as an internal standard. The plasma samples were subjected to a suitable sample clean-up consisting of a simple and relatively fast, two step liquid–liquid ion-pair extraction procedure. The chromatography, using the same volatile ion-pair reagent heptafluorobutyric acid (HFBA), takes only 10
min. Relative standard deviation of retention times was never above 2.26% (
n
=
36). The method was fully validated based on the US FDA Bioanalytical Method Validation Guidance for Industry. As such, a quantitative ESI-LC–MS(/MS) (TOF mass spectrometry) method was optimized for the absolute quantification of glycopyrrolate in human plasma in a concentration range from 0.101 to 101
ng/mL using a quadratic calibration function (
R
2
=
0.9995),
y
=
−2.21
×
10
−4 (±3.93
×
10
−5)
×
x
2
+
5.85
×
10
−2 (±5.27
×
10
−3)
×
x
+
4.08
×
10
−3 (±4.82
×
10
−4). For the three QC concentrations (QC
1 0.252, QC
2 2.52, and QC
3 25.2
ng/mL) and the LLOQ (0.101
ng/mL), total precision was under 20% (18.0% (
n
=
6) at the LLOQ) and maximum accuracy was 112% (88.9% for the LLOQ,
n
=
6). Absolute matrix effect (maximum 133%
±
9.59,
n
=
3), absolute recovery (better than 41.8%
±
2.22,
n
=
3), relative (inter-subject) matrix effect (maximum 10.9%
±
1.45,
n
=
4) and process efficiency (better than 45.2%
±
5.74,
n
=
3) too were assessed at the 3 QC concentrations.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>18977186</pmid><doi>10.1016/j.jchromb.2008.10.013</doi><tpages>7</tpages><oa>free_for_read</oa></addata></record> |
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source | MEDLINE; Access via ScienceDirect (Elsevier) |
subjects | Analysis Analytical, structural and metabolic biochemistry Biological and medical sciences Chemical Fractionation - methods Chromatography, High Pressure Liquid - methods Fundamental and applied biological sciences. Psychology General pharmacology Glycopyrrolate Glycopyrrolate - blood Humans LC–MS/MS Medical sciences Pharmacokinetics Pharmacology. Drug treatments Reproducibility of Results Spectrometry, Mass, Electrospray Ionization - methods Tandem Mass Spectrometry - methods |
title | Quantitative determination of glycopyrrolate in human plasma by liquid chromatography–electrospray ionization mass spectrometry: The use of a volatile ion-pairing agent during both liquid–liquid extraction and liquid chromatography |
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