UPLC-MS/MS Analysis of Methotrexate in Human Plasma and Comparison with the Fluorescence Polarization Immunoassay

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  • MEI Shenghui
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University
  • ZHU Leting
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University
  • LI Xingang
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University
  • WANG Jiaqing
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University
  • JIANG Xueyun
    Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University
  • CHEN Haiyan
    Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University
  • HUO Jiping
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University
  • YANG Li
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University
  • LIN Song
    Department of Neurosurgery, Beijing Tiantan Hospital, Capital Medical University
  • ZHAO Zhigang
    Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University Department of Clinical Pharmacology, College of Pharmaceutical Sciences, Capital Medical University

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抄録

Methotrexate (MTX) plasma concentration is routinely monitored to guide the dosage regimen of rescue drugs. This study aims to develop and validate an ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for plasma MTX analysis, and to establish its agreement with the fluorescence polarization immunoassay (FPIA) in patients with high-dose MTX therapy. Separation was achieved by gradient elution with methanol and water (0.05% formic acid) at 40°C with a run time of 3 min. The intra- and inter-day inaccuracy and imprecision of the UPLC-MS/MS method were –4.25 to 3.1 and less than 7.63%, respectively. The IS-normalized recovery and matrix effect were 87.05 to 92.81 and 124.43 to 134.57%. The correlation coefficients between UPLC-MS/MS and FPIA were greater than 0.98. The UPLC-MS/MS method was in agreement with the FPIA at high levels of MTX (1.0 – 100 μmol/L), but not at low levels (0.01 – 1.0 μmol/L). Further studies are warranted to confirm these results.

収録刊行物

  • Analytical Sciences

    Analytical Sciences 33 (6), 665-670, 2017

    社団法人 日本分析化学会

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