| 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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MedLine Citation:
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PMID: 18977186 Owner: NLM Status: MEDLINE |
Abstract/OtherAbstract:
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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 x 10(-4) (+/-3.93 x 10(-5))xx(2)+5.85 x 10(-2) (+/-5.27 x 10(-3))xx+4.08 x 10(-3) (+/-4.82 x 10(-4)). For the three QC concentrations (QC(1) 0.252, QC(2) 2.52, and QC(3) 25.2ng/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. |
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Authors:
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M L Storme; R S t'Kindt; W Goeteyn; K Reyntjens; J F Van Bocxlaer |
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Publication Detail:
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Type: Journal Article; Research Support, Non-U.S. Gov't; Validation Studies Date: 2008-10-14 |
Journal Detail:
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Title: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Volume: 876 ISSN: 1570-0232 ISO Abbreviation: J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. Publication Date: 2008 Dec |
Date Detail:
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Created Date: 2008-11-25 Completed Date: 2009-02-19 Revised Date: - |
Medline Journal Info:
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Nlm Unique ID: 101139554 Medline TA: J Chromatogr B Analyt Technol Biomed Life Sci Country: Netherlands |
Other Details:
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Languages: eng Pagination: 24-30 Citation Subset: IM |
Affiliation:
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Laboratory of Medical Biochemistry and Clinical Analysis, Faculty of Pharmaceutical Sciences, Ghent University, Harelbekestraat 72, Ghent, Belgium. |
Export Citation:
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| MeSH Terms | |
Descriptor/Qualifier:
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Chemical Fractionation
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methods* Chromatography, High Pressure Liquid / methods* Glycopyrrolate / blood* Humans Reproducibility of Results Spectrometry, Mass, Electrospray Ionization / methods* Tandem Mass Spectrometry / methods |
| Chemical | |
Reg. No./Substance:
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596-51-0/Glycopyrrolate |
From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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