Development of a novel ion-pairing UPLC method with cation-exchange solid-phase extraction for determination of free timolol in human plasma

Anthony Gallegos, Thomas Peavy, Roy Dixon, Roslyn Rivkah Isseroff

Research output: Contribution to journalArticle

2 Citations (Scopus)

Abstract

A novel UPLC-UV method was developed for analysis of timolol in human plasma using a simple, fast, and cost effective ion-exchange SPE procedure, followed by separation on a C18 UPLC column with a mobile phase consisting of acetonitrile, phosphate buffer, and sodium 1-octane sulfonate as an ion pairing agent. The method was fully validated according to US-FDA guidelines, and was found to be sufficiently accurate and precise for analysis of timolol in human plasma for clinical pharmacokinetic studies. The application of ion-exchange SPE cartridges for purification of timolol in plasma produced excellent percent recoveries and good sample clean-up, while the ion-pairing separation described here allowed quantitation of timolol without interference from endogenous sample components. The method lower limit of detection was 1.7 ng/mL and the lower limit of quantitation was 5.0 ng/mL, allowing for analysis of therapeutic concentrations of timolol in plasma.

Original languageEnglish (US)
Pages (from-to)228-235
Number of pages8
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume1096
DOIs
StatePublished - Oct 1 2018

Fingerprint

Plasma (human)
Timolol
Solid Phase Extraction
Cations
Ion exchange
Ions
Ion Exchange
Plasmas
Pharmacokinetics
Purification
Limit of Detection
Buffers
Sodium
Phosphates
Guidelines
Costs and Cost Analysis
Recovery
Costs

Keywords

  • Ion-exchange
  • Ion-pairing chromatography
  • Liquid chromatography
  • Plasma
  • Solid-phase extraction
  • Timolol

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Clinical Biochemistry
  • Cell Biology

Cite this

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title = "Development of a novel ion-pairing UPLC method with cation-exchange solid-phase extraction for determination of free timolol in human plasma",
abstract = "A novel UPLC-UV method was developed for analysis of timolol in human plasma using a simple, fast, and cost effective ion-exchange SPE procedure, followed by separation on a C18 UPLC column with a mobile phase consisting of acetonitrile, phosphate buffer, and sodium 1-octane sulfonate as an ion pairing agent. The method was fully validated according to US-FDA guidelines, and was found to be sufficiently accurate and precise for analysis of timolol in human plasma for clinical pharmacokinetic studies. The application of ion-exchange SPE cartridges for purification of timolol in plasma produced excellent percent recoveries and good sample clean-up, while the ion-pairing separation described here allowed quantitation of timolol without interference from endogenous sample components. The method lower limit of detection was 1.7 ng/mL and the lower limit of quantitation was 5.0 ng/mL, allowing for analysis of therapeutic concentrations of timolol in plasma.",
keywords = "Ion-exchange, Ion-pairing chromatography, Liquid chromatography, Plasma, Solid-phase extraction, Timolol",
author = "Anthony Gallegos and Thomas Peavy and Roy Dixon and Isseroff, {Roslyn Rivkah}",
year = "2018",
month = "10",
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T1 - Development of a novel ion-pairing UPLC method with cation-exchange solid-phase extraction for determination of free timolol in human plasma

AU - Gallegos, Anthony

AU - Peavy, Thomas

AU - Dixon, Roy

AU - Isseroff, Roslyn Rivkah

PY - 2018/10/1

Y1 - 2018/10/1

N2 - A novel UPLC-UV method was developed for analysis of timolol in human plasma using a simple, fast, and cost effective ion-exchange SPE procedure, followed by separation on a C18 UPLC column with a mobile phase consisting of acetonitrile, phosphate buffer, and sodium 1-octane sulfonate as an ion pairing agent. The method was fully validated according to US-FDA guidelines, and was found to be sufficiently accurate and precise for analysis of timolol in human plasma for clinical pharmacokinetic studies. The application of ion-exchange SPE cartridges for purification of timolol in plasma produced excellent percent recoveries and good sample clean-up, while the ion-pairing separation described here allowed quantitation of timolol without interference from endogenous sample components. The method lower limit of detection was 1.7 ng/mL and the lower limit of quantitation was 5.0 ng/mL, allowing for analysis of therapeutic concentrations of timolol in plasma.

AB - A novel UPLC-UV method was developed for analysis of timolol in human plasma using a simple, fast, and cost effective ion-exchange SPE procedure, followed by separation on a C18 UPLC column with a mobile phase consisting of acetonitrile, phosphate buffer, and sodium 1-octane sulfonate as an ion pairing agent. The method was fully validated according to US-FDA guidelines, and was found to be sufficiently accurate and precise for analysis of timolol in human plasma for clinical pharmacokinetic studies. The application of ion-exchange SPE cartridges for purification of timolol in plasma produced excellent percent recoveries and good sample clean-up, while the ion-pairing separation described here allowed quantitation of timolol without interference from endogenous sample components. The method lower limit of detection was 1.7 ng/mL and the lower limit of quantitation was 5.0 ng/mL, allowing for analysis of therapeutic concentrations of timolol in plasma.

KW - Ion-exchange

KW - Ion-pairing chromatography

KW - Liquid chromatography

KW - Plasma

KW - Solid-phase extraction

KW - Timolol

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