Personalized monitoring of therapeutic salicylic acid in dried blood spots using a three-layer setup and desorption electrospray ionization mass spectrometry

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• 作者：Markus Siebenhaar ; Kai Küllmer…
• 关键词：Desorption electrospray ionization ; Three ; layer method ; Quantification ; Salicylic acid ; Ambient mass spectrometry ; Therapeutic drug monitoring
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2015
• 出版时间：September 2015
• 年：2015
• 卷：407
• 期：23
• 页码：7229-7238
• 全文大小：538 KB
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• 作者单位：Markus Siebenhaar (1) (2) (3)
  Kai Küllmer (3)
  Nuno Miguel de Barros Fernandes (3)
  Volker Hüllen (3)
  Carsten Hopf (1) (2)
  
  1. Instrumental Analysis and Bioanalysis, Department of Biotechnology, Mannheim University of Applied Sciences, Paul-Wittsack-Str. 10, 68163, Mannheim, Germany
  2. Institute of Medical Technology, University of Heidelberg and Mannheim University of Applied Sciences, Paul-Wittsack-Str. 10, 68163, Mannheim, Germany
  3. Roche Diabetes Care GmbH, Sandhofer Stra?e 116, 68305, Mannheim, Germany
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

Desorption electrospray ionization (DESI) mass spectrometry is an emerging technology for direct therapeutic drug monitoring in dried blood spots (DBS). Current DBS methods require manual application of small molecules as internal standards for absolute drug quantification. With industrial standardization in mind, we superseded the manual addition of standard and built a three-layer setup for robust quantification of salicylic acid directly from DBS. We combined a dioctyl sodium sulfosuccinate weave facilitating sample spreading with a cellulose layer for addition of isotope-labeled salicylic acid as internal standard and a filter paper for analysis of the standard-containing sample by DESI-MS. Using this setup, we developed a quantification method for salicylic acid from whole blood with a validated linear curve range from 10 to 2000 mg/L, a relative standard deviation (RSD%) ?4 %, and determination coefficients of 0.997. The limit of detection (LOD) was 8 mg/L and the lower limit of quantification (LLOQ) was 10 mg/L. Recovery rates in method verification by LC-MS/MS were 97 to 101 % for blinded samples. Most importantly, a study in healthy volunteers after administration of a single dose of Aspirin provides evidence to suggest that the three-layer setup may enable individual pharmacokinetic and endpoint testing following blood collection by finger pricking by patients at home. Taken together, our data suggests that DBS-based quantification of drugs by DESI-MS on pre-manufactured three-layer cartridges may be a promising approach for future near-patient therapeutic drug monitoring. Keywords Desorption electrospray ionization Three-layer method Quantification Salicylic acid Ambient mass spectrometry Therapeutic drug monitoring