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<p>In this work, the manual multistep QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach has been streamlined into an in-syringe micro-QuEChERS method, referred to as an in-syringe-assisted fast drug extraction (IS-FaDEx) coupled with semi-automated (SA) dispersive solid-phase cleanup (dSPC), for fast quantification of direct oral anticoagulant drugs (DOACs) in human plasma samples using ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) detection. In the IS-FaDEx-SA-dSPC method, 100 µL of plasma was taken into a 3-mL plastic syringe for salt-induced liquid–liquid extraction, after which the extractant was transferred to another 3-mL plastic syringe for the dSPC procedure using sorbents with salt (including C18, sorbent with primary-secondary amine functionalities, and anhydrous MgSO<sub>4</sub>), and the final clean extractant was injected into UHPLC-MS/MS for analysis. Experimental factors affecting the extraction efficiency of DOACs, including extraction solvent, salt type and amount, and cleanup sorbent type and amount, were tested and optimized. Good linearity was observed over a calibration concentration range from 0.1 to 500&#xa0;µg&#xa0;mL<sup>−1</sup>, with correlation coefficients &gt; 0.99. Detection limits ranged between 0.02 and 0.1&#xa0;µg&#xa0;mL<sup>−1</sup>, and the intra- and inter-day (<i>n</i> = 6) relative standard deviations were &lt; 6%. As a proof of concept, the developed method was applied in real time to determine DOACs in plasma samples from patients with atrial fibrillation, demonstrating&#xa0;good accuracy,&#xa0;and good precision (spiked recoveries ranging from 85.3% to 105.3%). This method provides a simple, efficient, sensitive, and automated procedure for extracting and determining DOACs from plasma samples, which can serve as an alternative analytical tool for biomonitoring of DOACs in routine clinical laboratory practice, in particular in patients with atrial fibrillation and venous thromboembolism.</p> Graphical Abstract <p></p>

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A streamlined in-syringe fast drug extraction and semi-automated dispersive cleanup technique for quick biomonitoring of direct oral anti-coagulant drugs in patients’ plasma samples using UHPLC-MS/MS analysis

  • 期刊论文

  • 发表日期：

    2026年3月5日

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  • Shih-Tao Hu,
  • Swapnil Gurrani,
  • Cheng-Te Huang,
  • Karthikeyan Prakasham,
  • Tzu-Yu Pan,
  • Ming-Tsang Wu,
  • Po-Chin Huang,
  • Yu-Chia Lin,
  • Vinoth Kumar Ponnusamy,
  • Tsai-Hui Duh

摘要

In this work, the manual multistep QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach has been streamlined into an in-syringe micro-QuEChERS method, referred to as an in-syringe-assisted fast drug extraction (IS-FaDEx) coupled with semi-automated (SA) dispersive solid-phase cleanup (dSPC), for fast quantification of direct oral anticoagulant drugs (DOACs) in human plasma samples using ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) detection. In the IS-FaDEx-SA-dSPC method, 100 µL of plasma was taken into a 3-mL plastic syringe for salt-induced liquid–liquid extraction, after which the extractant was transferred to another 3-mL plastic syringe for the dSPC procedure using sorbents with salt (including C18, sorbent with primary-secondary amine functionalities, and anhydrous MgSO4), and the final clean extractant was injected into UHPLC-MS/MS for analysis. Experimental factors affecting the extraction efficiency of DOACs, including extraction solvent, salt type and amount, and cleanup sorbent type and amount, were tested and optimized. Good linearity was observed over a calibration concentration range from 0.1 to 500 µg mL−1, with correlation coefficients > 0.99. Detection limits ranged between 0.02 and 0.1 µg mL−1, and the intra- and inter-day (n = 6) relative standard deviations were < 6%. As a proof of concept, the developed method was applied in real time to determine DOACs in plasma samples from patients with atrial fibrillation, demonstrating good accuracy, and good precision (spiked recoveries ranging from 85.3% to 105.3%). This method provides a simple, efficient, sensitive, and automated procedure for extracting and determining DOACs from plasma samples, which can serve as an alternative analytical tool for biomonitoring of DOACs in routine clinical laboratory practice, in particular in patients with atrial fibrillation and venous thromboembolism.

Graphical Abstract