Rapid and high-throughput screening of multi-residue pharmaceutical drugs in bovine tissue using solid phase microextraction and direct analysis in real time-tandem mass spectrometry (SPME-DART-MS/MS)

Abstract

Direct Analysis in Real Time (DART) has become a popular research area in food safety monitoring due to its unique characteristics that allow rapid and high-throughput screening of complex matrices with minimal sample preparation. The current research aimed to investigate the detection and quantitation capabilities of solid phase microextraction (SPME) and DART coupled to tandem mass spectrometry MS/MS for a large number of pharmaceutical drugs covering a wide range of physico-chemical properties (log P, -1.22-5.97) in complex animal-food matrices such as beef tissue. 53% of the 98 target analytes selected initially could be efficiently ionized by DART and quantified at or below the Canadian maximum residue limits (MRLs) and US regulatory tolerances in bovine muscle. Despite using only two internal standards for correction, promising results were obtained for these analytes, where 62% of the detected analytes achieved linear correlation coefficients >0.99 within the evaluated range of concentrations (0.25-3X, where X corresponds to the MRL for each target analyte). In addition, more than 92% of the detected analytes achieved average accuracies within the 70-120% range of their true concentrations and intraday repeatability RSDs ≤25% at the 0.5X, 1X, and 2X concentration levels. The fully automated sample preparation workflow allowed for total extraction and analysis times as short as 1 min time per sample. While DART has limited capabilities in terms of analyte coverage, this research highlights the potential usefulness of SPME-DART-MS/MS as a method for rapid analysis in food safety monitoring applications.

Keywords: Direct analysis in real time; High-throughput analysis; Multi-residue veterinary drug analysis; Rapid analysis; Solid phase microextraction.