Quantification of Saquinavir from Lysates of Peripheral Blood Mononuclear Cells Using Microarrays and Standard MALDI-TOF-MS

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• 作者：Martin Pabst (1)
  Stephan Rupert Fagerer (1)
  Rudolf K?hling (2)
  Klaus Eyer (1)
  Jasmin Krismer (1)
  Konstantins Jefimovs (3)
  Alfredo Jesus Ibá?ez (1)
  Renato Zenobi (1)
  
• 关键词：Quantitative MALDI ; MS ; Saquinavir ; Cell lysate analysis ; Peripheral blood mononuclear cells ; Microarrays for mass spectrometry (MAMS) ; Antiretroviral drugs
• 刊名：Journal of The American Society for Mass Spectrometry
• 出版年：2014
• 出版时间：June 2014
• 年：2014
• 卷：25
• 期：6
• 页码：1083-1086
• 全文大小：
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• 作者单位：Martin Pabst (1)
  Stephan Rupert Fagerer (1)
  Rudolf K?hling (2)
  Klaus Eyer (1)
  Jasmin Krismer (1)
  Konstantins Jefimovs (3)
  Alfredo Jesus Ibá?ez (1)
  Renato Zenobi (1)
  
  1. Department of Chemistry and Applied Biosciences, ETH Zürich, 8093, Zürich, Switzerland
  2. Sigma-Aldrich, 9470, Buchs, Switzerland
  3. Swiss Federal Laboratories for Material Science and Technology EMPA, 8600, Dübendorf, Switzerland
  
• ISSN：1879-1123

文摘

Drug monitoring is usually performed by liquid chromatography coupled with optical detection or electrospray ionization mass spectrometry. More recently, matrix-assisted laser desorption/ionization (MALDI) in combination with triple quadrupole or Fourier-transform (FT) mass analyzers has also been reported to allow accurate quantification. Here, we present a strategy that employs standard MALDI time-of-flight (TOF) mass spectrometry (MS) for the sensitive and accurate quantification of saquinavir from an extract of blood peripheral mononuclear cells. Unambiguous identification of saquinavir in the mass spectra was possible because of using internal mass calibration and by an overall low chemical noise in the low mass range. Exact mass determination of the constant background peaks of the cell extract, which were used for recalibration, was performed by an initial MALDI-FT-MS analysis. Fast and multiplexed sample analysis was enabled by microarray technology, which provided 10 replicates in the lower nL range for each sample in parallel lanes on a chip. In order to validate the method, we employed various statistical tests, such as confidence intervals for linear regressions, three quality control samples, and inverse confidence limits of the estimated concentration ratios. Figure ?/div>