The analysis of β-agonists by packed-column supercritical fluid chromatography with ultra-violet and atmospheric pressure chemical ionisation mass spectrometric detection

David C. Jones, Kenan Dost, George Davidson, Michael W. George

Research output: Journal PublicationArticlepeer-review

31 Citations (Scopus)

Abstract

Packed-column supercritical fluid chromatography (pSFC) using ultra-violet (UV) and atmospheric pressure chemical ionisation (APCI) mass spectrometry (MS) provides a versatile method for the identification and quantification of β-agonists. We have achieved good separation of clenbuterol, salbutamol, terbutaline and fenoterol with good resolution and reasonable retention times using a high concentration of methanol modifier in the supercritical CO2, together with small amounts of both acidic (trifluroacetic acid, TFAA) and basic (triethylamine, TEA, or diethylamine, DEA) additives. APCI-MS gave unambiguous identification of the 4 analytes, and increasing cone voltage provided informative fragmentation patterns. The pSFC-MS technique was shown to be linear (R2 ≥ 0.996) over the concentration range 1-50 μg ml-1. Single ion monitoring (SIM) gave detection limits (on-column) of 2.5 ng (clenbuterol), 0.83 ng (terbutaline), 7.6 ng (salbutamol) and 2.7 ng (fenoterol). The pSFC-MS system was shown to be reproducible within a day, between days, and between restrictors. Analysis of milk samples 'spiked' with β-agonists showed that the matrix caused no interference, with detection limits of approximately 500 μg l-1 of β-agonists. More dilute solutions could be analysed by pre-concentration before the SFC stage.

Original languageEnglish
Pages (from-to)827-831
Number of pages5
JournalThe Analyst
Volume124
Issue number6
DOIs
Publication statusPublished - 1999
Externally publishedYes

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Environmental Chemistry
  • Spectroscopy
  • Electrochemistry

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