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采用固相微萃取-实时直接分析-串联质谱法(SPME-DART-MS/MS)快速高通量筛选牛组织中的多残留药物。

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).

机构信息

Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada.

Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada; On Leave from Institute of Chemistry, University of Campinas, Campinas, São Paulo, 13083-970, Brazil.

出版信息

Talanta. 2020 Sep 1;217:121095. doi: 10.1016/j.talanta.2020.121095. Epub 2020 Apr 30.

DOI:10.1016/j.talanta.2020.121095
PMID:32498882
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.

摘要

直接分析实时技术 (DART) 因其独特的特点,在食品安全监测领域已成为一个热门的研究领域,这些特点包括可快速、高通量筛选复杂基质,且样品制备量最小。本研究旨在调查固相微萃取 (SPME) 和 DART 与串联质谱 MS/MS 结合用于检测和定量分析复杂动物食品基质(如牛肉组织)中大量药物的能力,这些药物涵盖了广泛的物理化学性质 (log P,-1.22-5.97)。最初选择的 98 个目标分析物中有 53%可被 DART 有效离子化,并在加拿大最大残留限量 (MRL) 以下或美国监管容忍度以下定量检测到牛肌肉中的分析物。尽管仅使用了两种内标物进行校正,但这些分析物仍获得了有前景的结果,其中 62%的检测到的分析物在评估浓度范围内 (0.25-3X,其中 X 对应于每个目标分析物的 MRL) 获得了 >0.99 的线性相关系数。此外,超过 92%的检测到的分析物在其真实浓度的 70-120%范围内达到了平均准确度,并且在 0.5X、1X 和 2X 浓度水平下,日内重复性 RSDs ≤25%。全自动样品制备工作流程允许每个样品的总提取和分析时间最短为 1 分钟。虽然 DART 在分析物覆盖范围方面能力有限,但本研究强调了 SPME-DART-MS/MS 作为食品安全监测应用中快速分析方法的潜在用途。

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