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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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MLA
Storme, ML 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.
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.
Chicago author-date
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.
Chicago author-date (all authors)
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.
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.
IEEE
[1]
M. Storme, R. T’Kindt, W. Goeteyn, K. REYNTJENS, and J. Van Bocxlaer, “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, vol. 876, no. 1, pp. 24–30, 2008.
@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},
  keywords     = {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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