Determination of methotrexate in environmental samples by solid phase extraction and high performance liquid chromatography: Ultraviolet or tandem mass spectrometry detection?

Research output: Contribution to journalArticle

Abstract

In order to assess exposure levels of hospital personnel involved in the preparation and administration of antineoplastic drugs, environmental monitoring should be carried out. Wipe samples, pads, gloves and air samples should be collected at the end of each work shift, properly treated and then analysed using instrumental techniques which are sufficiently sensitive and specific to detect even trace amounts of drug. In this study, a method using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), incorporating solid phase extraction (SPE), was validated for determination of methotrexate (MTX) in wipe and air samples. Each step of the method was first developed and optimised using ultraviolet detection (UV), and afterwards tandem mass spectrometry was used to obtain a lower limit of quantitation when the expected drug level was less than the analytical UV detection limit. SPE enabled a 20-fold preconcentration of the analyte when using HPLC/UV and a further 30-fold preconcentration was obtained when analysing samples by HPLC/MS/MS. For example, the limit of quantitation (LLQ) was lowered from 3000 ng on wipe (direct injection onto an HPLC/UV system) to 5 ng on wipe (SPE plus HPLC/MS/MS). 7-hydroxymethotrexate was used as internal standard to assess precision and accuracy. Copyright (C) 2000 John Wiley and Sons, Ltd.

Original languageEnglish
Pages (from-to)685-691
Number of pages7
JournalRapid Communications in Mass Spectrometry
Volume14
Issue number8
DOIs
Publication statusPublished - 2000

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High performance liquid chromatography
Methotrexate
Mass spectrometry
7-hydroxymethotrexate
Direct injection
Air
Pharmaceutical Preparations
Antineoplastic Agents
Personnel
Monitoring

ASJC Scopus subject areas

  • Analytical Chemistry
  • Spectroscopy

Cite this

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title = "Determination of methotrexate in environmental samples by solid phase extraction and high performance liquid chromatography: Ultraviolet or tandem mass spectrometry detection?",
abstract = "In order to assess exposure levels of hospital personnel involved in the preparation and administration of antineoplastic drugs, environmental monitoring should be carried out. Wipe samples, pads, gloves and air samples should be collected at the end of each work shift, properly treated and then analysed using instrumental techniques which are sufficiently sensitive and specific to detect even trace amounts of drug. In this study, a method using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), incorporating solid phase extraction (SPE), was validated for determination of methotrexate (MTX) in wipe and air samples. Each step of the method was first developed and optimised using ultraviolet detection (UV), and afterwards tandem mass spectrometry was used to obtain a lower limit of quantitation when the expected drug level was less than the analytical UV detection limit. SPE enabled a 20-fold preconcentration of the analyte when using HPLC/UV and a further 30-fold preconcentration was obtained when analysing samples by HPLC/MS/MS. For example, the limit of quantitation (LLQ) was lowered from 3000 ng on wipe (direct injection onto an HPLC/UV system) to 5 ng on wipe (SPE plus HPLC/MS/MS). 7-hydroxymethotrexate was used as internal standard to assess precision and accuracy. Copyright (C) 2000 John Wiley and Sons, Ltd.",
author = "Roberta Turci and Giuseppina Micoli and Claudio Minoia",
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