HYDROPHILIC INTERACTION CHROMATOGRAPHY COMBINED WITH TANDEM-MASS SPECTROMETRY FOR QUANTITATIVE DETERMINATION OF SIX AMINOGLYCOSIDE ANTIMICROBIALS IN HUMAN PLASMA

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  • OMIYA Shinya
    Department of Legal Medicine, Showa University School of Medicine Department of Medicine, Division of Nephrology, Showa University Fujigaoka Hospital
  • KUMAZAWA Takeshi
    Department of Legal Medicine, Showa University School of Medicine
  • LEE Xiao-Pen
    Department of Legal Medicine, Showa University School of Medicine
  • SHOJI Yukiko
    Department of Legal Medicine, Showa University School of Medicine
  • SATO Junichi
    Department of Legal Medicine, Showa University School of Medicine
  • SAWAGUCHI Toshiko
    Department of Legal Medicine, Showa University School of Medicine National Institute of Public Health
  • YOSHIMURA Ashio
    Department of Medicine, Division of Nephrology, Showa University Fujigaoka Hospital
  • SATO Keizo
    Department of Legal Medicine, Showa University School of Medicine

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Other Title
  • HILIC-MS-MSによる血漿中アミノグリコシド系抗菌薬の簡易迅速分析法
  • HILIC-MS-MS ニ ヨル ケッショウ チュウ アミノグリコシドケイ コウキンヤク ノ カンイ ジンソク ブンセキホウ

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A simple and rapid method was developed for the analysis of six aminoglycoside antimicrobials (streptomycin, ribostamycin, kanamycin, amikacin, dibekacin, arbekacin) in human plasma samples using hydrophilic interaction liquid chromatography (HILIC)-tandem mass spectrometry (MS-MS). A small volume of plasma (50µl) spiked with the 10µl of standard solution containing the test drugs and 10µl of internal standard solution was diluted with 430µl of purified water/0.1% formic acid in acetonitrile (1:3, v/v). After centrifugation of the mixture, the supernatant extract was directly injected into the HILIC-MS-MS, without any solvent evaporation or reconstitution steps. The analytes were separated on an Inertsil Amide metal-free PEEK column (50×2.1mm i.d., particle size 3µm) using a gradient with 0.1% formic acid in purified water and 0.1% formic acid in acetonitrile at a flow of 0.6ml/min. All drugs showed base peaks due to ［M＋H］＋ ions by HILIC-MS with positive ion electrospray ionization, and the product ions were produced from each ［M＋H］＋ ion by HILIC-MS-MS. Quantitation was performed by selective reaction monitoring using each base peak of product ions of HILIC-MS-MS. Good peak shapes of the six drugs were achieved within an analysis time of 1.4 min. All drugs spiked into the plasma showed recoveries of 23-77% and extraction efficiencies of 72-105%. The regression equations for the antimicrobials showed excellent linearity with the limits of quantitation of 3.9-16µg/ml. The intra- and inter-day relative standard deviations for all drugs were not greater than 19%. The accuracies of quantitation were 80-114%. Streptomycin and kanamycin in human plasma after intramuscular administration of the drugs could actually be determined. This method appears to be useful for determining aminoglycoside antimicrobials in human plasma in clinical and forensic investigations.

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