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Volume 33 Issue 2
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Article Navigation >  Journal of Pharmaceutical Practice and Service  > 2015  >  33(2): 143-146,158

WANG Yixuan, WU Dan, CAO Junning, QIAN Jun. Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(2): 143-146,158. doi: 10.3969/j.issn.1006-0111.2015.02.013
Citation: WANG Yixuan, WU Dan, CAO Junning, QIAN Jun. Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(2): 143-146,158. doi: 10.3969/j.issn.1006-0111.2015.02.013
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Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry

doi: 10.3969/j.issn.1006-0111.2015.02.013

  • Department of Medical Oncology, Cancer Hospital Affilliated to Fudan University; Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032, China

  • Received Date: 2014-04-03
  • Rev Recd Date: 2014-06-26
  • Objective To develop an SPE-HPLC method for the determination of methotrexate (MTX) in human plasma to monitor the clinical drug use of MTX, and to identify the human metabolite of MTX by mass spectrometry. Methods MTX was extracted from human plasma using C18 SPE column and analyzed directly after elution. The separation of MTX was performed on Diamonsil C18 column (150 mm×4.6 mm, 5 m) with a gradient mobile phase of methanol and 0.5% acetic acid solution (containing 0.3% triethylamine) at a flow rate of 1.0 ml/min. The detection wavelength was 306 nm. QLMS and MRM-IDA-EPI scan modes were used to obtain the mass spectrum of MTX metabolite. Results The calibration curve of MTX in plasma was linear over the range of 0.05-100 μmol/L(r=0.999 9). The extraction recovery was above 95% and accuracy was between 97% and 105%. Both intra-and inter-day precision were less than 5%. 7-OH MTX was identified to be the metabolite through the analysis of the mass spectrum. Conclusion The method is sensitive, reproducible, easy to operate and suits for monitoring the concentration of MTX in clinical practice.
  • [1] Green MR,Chowdhary S,Lombardi KM,et al.Clinical utility and pharmacology of high-dose MTX in the treatment of primary CNS lymphoma[J].Expert Rev Neurother,2006,6(5):635-652.
    [2] Lennard L.Therapeutic drug monitoring of antimetabolic cytotoxic drugs[J].Br J Clin Pharmacol,1999,47:131-143.
    [3] 彭 波.高效液相色谱法测定甲氨蝶呤的血药浓度[J].中国医院药学杂志,2011, 31 (11):951-952.
    [4] 张春燕,顾 健.反相高效液相色谱法同时测定人血浆中亚叶酸、5-甲基四氢叶酸及甲氨蝶呤的浓度及临床应用[J].中国药学杂志,2010,45(7):543-547.
    [5] 许耘川,袁向亮,沈立松.HPLC法测定血清甲氨蝶呤浓度的方法建立及其与荧光偏振法的比较[J].检验医学,2010,25(9):701-704.
    [6] 谢军平,冯玲玲,匡 霞.HPLC 测定大剂量甲氨蝶呤患者血药浓度[J].中国实验方剂学杂志,2010,16(11):69-72.
    [7] 霍 晶,袁盛华,方 芸,等.反相高效液相色谱法测定人血浆中甲氨蝶呤的浓度[J].药学与临床研究,2007,15(5):390-392.
    [8] Turci R,Micoli G,Minoia C.Determination of methotrexate in environmental samples by solid phase extraction and high performance liquid chromatography: ultraviolet or tandem mass spectrometry detection?[J].Rapid Commun Mass Spectr,2000,14:685-691.
    [9] 周 卿,潘雪君.固相萃取-高效液相色谱法测定人乳中甲氨蝶呤的含量[J].药物分析杂志,2011,31(12):2305-2307.
    [10] 吴雪梅, 丘宏强, 方令平, 等.固相萃取-高效液相色谱法测定甲氨蝶呤的血药浓度[J].中国医院药学杂志,2008,28(18):1617-1619.
    [JP2]张华年,文玲莉,张少文, 等.固相萃取高效液相色谱法检测生物样本中甲氨喋呤[J].药物分析杂志,2000,20(6):401-404.
    [12] 曹一辰,孟祥乐,朱金辉,等.LC-MS/MS法测定人血清中甲氨蝶呤及其代谢产物7-羟基甲氨蝶呤的浓度[J].中国药师,2012,15(2):191-194.
    [13] Guo PI, Wang XM, Liu LS, et al.Determination of methotrexate and its major metabolite 7-hydroxymethotrexate in mouse plasma and brain tissue by liquid chromatography-tandem mass spectrometry[J].J Pharm Biomed Anal,2007,43:1789-1795.
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Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry

doi: 10.3969/j.issn.1006-0111.2015.02.013
  • Department of Medical Oncology, Cancer Hospital Affilliated to Fudan University; Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032, China
  • Received Date: 2014-04-03
  • Rev Recd Date: 2014-06-26

Abstract: Objective To develop an SPE-HPLC method for the determination of methotrexate (MTX) in human plasma to monitor the clinical drug use of MTX, and to identify the human metabolite of MTX by mass spectrometry. Methods MTX was extracted from human plasma using C18 SPE column and analyzed directly after elution. The separation of MTX was performed on Diamonsil C18 column (150 mm×4.6 mm, 5 m) with a gradient mobile phase of methanol and 0.5% acetic acid solution (containing 0.3% triethylamine) at a flow rate of 1.0 ml/min. The detection wavelength was 306 nm. QLMS and MRM-IDA-EPI scan modes were used to obtain the mass spectrum of MTX metabolite. Results The calibration curve of MTX in plasma was linear over the range of 0.05-100 μmol/L(r=0.999 9). The extraction recovery was above 95% and accuracy was between 97% and 105%. Both intra-and inter-day precision were less than 5%. 7-OH MTX was identified to be the metabolite through the analysis of the mass spectrum. Conclusion The method is sensitive, reproducible, easy to operate and suits for monitoring the concentration of MTX in clinical practice.

WANG Yixuan, WU Dan, CAO Junning, QIAN Jun. Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(2): 143-146,158. doi: 10.3969/j.issn.1006-0111.2015.02.013
Citation: WANG Yixuan, WU Dan, CAO Junning, QIAN Jun. Determination of methotrexate in human plasma by HPLC and qualitative analysis of its metabolite by mass spectrometry[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(2): 143-146,158. doi: 10.3969/j.issn.1006-0111.2015.02.013
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