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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

ML Storme, Ruben T'Kindt (UGent) , Wim Goeteyn (UGent) , KOEN REYNTJENS (UGent) and Jan Van Bocxlaer (UGent)
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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 x 10(-4) (+/- 3.93 x 10(-5)) x chi(2) + 5.85 x 10(-2) (+/- 5.27 x 10(-3)) x x + 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) 25.2 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.
Keywords
DIQUAT, URINE, PARAQUAT, SAMPLE PRETREATMENT, CAPILLARY-ELECTROPHORESIS, SOLID-PHASE EXTRACTION, Pharmacokinetics, QUATERNARY AMMONIUM HERBICIDES, LC-MS/MS, Glycopyrrolate, COLUMN, SERUM, HPLC

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Chicago
Storme, ML, Ruben T’Kindt, Wim Goeteyn, KOEN REYNTJENS, and Jan Van Bocxlaer. 2008. “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.” Journal of Chromatography B-analytical Technologies in the Biomedical and Life Sciences 876 (1): 24–30.
APA
Storme, ML, T’Kindt, R., Goeteyn, W., REYNTJENS, K., & Van Bocxlaer, J. (2008). 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. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 876(1), 24–30.
Vancouver
1.
Storme M, T’Kindt R, Goeteyn W, REYNTJENS K, Van Bocxlaer J. 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. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES. PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS: ELSEVIER SCIENCE BV,; 2008;876(1):24–30.
MLA
Storme, ML, Ruben T’Kindt, Wim Goeteyn, et al. “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.” JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES 876.1 (2008): 24–30. Print.
@article{529437,
  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 x 10(-4) (+/- 3.93 x 10(-5)) x chi(2) + 5.85 x 10(-2) (+/- 5.27 x 10(-3)) x x + 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) 25.2 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.},
  author       = {Storme, ML and T'Kindt, Ruben and Goeteyn, Wim and REYNTJENS, KOEN and Van Bocxlaer, Jan},
  issn         = {1570-0232},
  journal      = {JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES},
  keyword      = {DIQUAT,URINE,PARAQUAT,SAMPLE PRETREATMENT,CAPILLARY-ELECTROPHORESIS,SOLID-PHASE EXTRACTION,Pharmacokinetics,QUATERNARY AMMONIUM HERBICIDES,LC-MS/MS,Glycopyrrolate,COLUMN,SERUM,HPLC},
  language     = {eng},
  number       = {1},
  pages        = {24--30},
  publisher    = {ELSEVIER SCIENCE BV,},
  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},
  url          = {http://dx.doi.org/10.1016/j.jchromb.2008.10.013},
  volume       = {876},
  year         = {2008},
}

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