Multi-residue determination of anti-inflammatory analgesics in sera by liquid chromatography-mass spectrometry

Irina Rudik Miksa, Margaret R. Cummings, Robert H Poppenga

Research output: Contribution to journalArticle

25 Citations (Scopus)

Abstract

Non-steroidal anti-inflammatories (NSAIDs) are analgesic, antipyretic, and, as their name implies, anti-inflammatory drugs, which are widely used for the treatment of a variety of human and veterinary disease conditions in which control of pain and inflammation is desired. Acetaminophen (ACE) is a common over-the-counter analgesic. Detection of a variety of widely used NSAIDs and ACE in fluid and tissue samples is an important diagnostic tool. A sensitive and selective analytical method has been developed for simultaneous screening of 12 NSAIDs and ACE by liquid chromatography-mass spectrometry with an atmospheric pressure chemical ionization interface set to operate in the negative ion mode of MS. Following sample preparation, all analytes were separated on a C18-reversed-phase column with a gradient elution of acetonitrile and acetic acid. Full-scan mass spectral fragmentation profiles were established for each analyte and individual extracted ion chromatograms were used for quantitation. Linearity of detection was observed over the 0.05-25.0 μg/mL range of standard concentrations. The instrument limits of detection (LOD), based on an individual analyte quantitation ions, fell between 0.05 and 1.0 μg/mL for all compounds. The matrix LODs were determined to be 0.05 μg/mL for phenylbutazone (m/z 307); 0.1 μg/mL for indomethacin (m/z 312), flunixin (m/z 295), and piroxicam (m/z 330); 0.5 μg/mL for ACE (m/z 150), diclofenac (m/z 250), ketoprofen (m/z 209), and mefenamic acid (m/z 240); 1.0 μg/mL for oxyphenbutazone (m/z 323); 5.0 μg/mL for ibuprofen (m/z 205), salicylic acid (m/z 137), and tolmetin (m/z 212); and 10 μg/mL for naproxen (m/z 185).

Original languageEnglish (US)
Pages (from-to)95-104
Number of pages10
JournalJournal of Analytical Toxicology
Volume29
Issue number2
StatePublished - Mar 2005
Externally publishedYes

Fingerprint

Liquid chromatography
Non-Steroidal Anti-Inflammatory Agents
Acetaminophen
Liquid Chromatography
Mass spectrometry
liquid chromatography
serum
Mass Spectrometry
mass spectrometry
Salicylic acid
ion
Ions
Acetonitrile
Serum
Acetic acid
Atmospheric pressure
Ionization
Analgesics
Screening
salicylic acid

ASJC Scopus subject areas

  • Analytical Chemistry
  • Toxicology
  • Health, Toxicology and Mutagenesis

Cite this

Multi-residue determination of anti-inflammatory analgesics in sera by liquid chromatography-mass spectrometry. / Miksa, Irina Rudik; Cummings, Margaret R.; Poppenga, Robert H.

In: Journal of Analytical Toxicology, Vol. 29, No. 2, 03.2005, p. 95-104.

Research output: Contribution to journalArticle

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