Development and validation of a sensitive LC-MS/MS method for the estimation of scopolamine in human serum

Suresh Kumar Swaminathan, James Fisher, Nicole K. Brogden, Karunya K. Kandimalla

Research output: Contribution to journalArticlepeer-review

2 Scopus citations

Abstract

Scopolamine is an anticholinergic alkaloid that is widely used in the form of a transdermal system to manage nausea associated with motion sickness. Currently available methods to quantify scopolamine require large sample volumes and involve cumbersome sample preparation. In this work, a simple method for the rapid separation and sensitive quantification of scopolamine in human serum was developed. Scopolamine was extracted from 0.5 mL of human serum using solid-phase extraction. The extracted samples were injected onto Zorbax XDB-C18 column (4.6 × 50 mm, 1.8 μm, and 600 bar) on an Agilent 1200 series HPLC. The chromatographic separation involved gradient elution with water and acetonitrile containing 0.1% v/v formic acid as a mobile phase. The samples were quantified in positive ion mode using a TSQ Quantum triple quadrupole mass spectrometer. The assay was validated and found to be linear over a concentration range of 5–5000 pg/mL. The total assay precision and accuracy was 6.3% and 96%, respectively. The lower limit of quantification (LLOQ) of the assay was 5 pg/mL. The assay was used in a human pharmacokinetic study to measure the concentration of scopolamine in serum after an administering scopolamine as transdermal delivery system or as an intravenous bolus dose.

Original languageEnglish (US)
Pages (from-to)41-46
Number of pages6
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume164
DOIs
StatePublished - Feb 5 2019

Bibliographical note

Funding Information:
We are grateful to the National Institute for Pharmaceutical Technology and Education (NIPTE) and the U.S. Food and Drug Administration (FDA) for providing funds for this research. This study was funded by the FDA Grant to NIPTE titled "The Critical Path Manufacturing Sector Research Initiative (U01)"; Grant 5U01FD004275 . All authors have no financial conflicts of interest.

Publisher Copyright:
© 2018

Keywords

  • Human serum
  • Liquid chromatography
  • Mass spectrometry
  • Scopolamine
  • Solid-phase extraction

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