A New Method to Quantify Ifosfamide Blood Levels Using Dried Blood Spots and UPLC-MS/MS in Paediatric Patients with Embryonic Solid Tumours

PLoS One. 2015 Nov 23;10(11):e0143421. doi: 10.1371/journal.pone.0143421. eCollection 2015.

Abstract

Ifosfamide blood concentrations are necessary to monitor its therapeutic response, avoiding any adverse effect. We developed and validated an analytical method by UPLC-MS/MS to quantify ifosfamide in dried blood spots (DBS). Blood samples were collected on Whatman 903® filter paper cards. Five 3 mm disks were punched out from each dried blood spot. Acetonitrile and ethyl acetate were used for drug extraction. Chromatographic separation was carried out in an Acquity UPLC equipment with a BEH-C18 column, 2.1 x 100 mm, 1.7 μm (Waters®). The mobile phase consisted in 5 mM ammonium formate and methanol:acetonitrile (40:48:12 v/v/v) at 0.2 mL/min. LC-MS/MS detection was done by ESI+ and multiple reaction mode monitoring, ionic transitions were m/z1+ 260.99 > 91.63 for ifosfamide and 261.00 > 139.90 for cyclophosphamide (internal standard). This method was linear within a 100-10000 ng/mL range and it was accurate, precise and selective. Ifosfamide samples in DBS were stable for up to 52 days at -80°C. The procedure was tested in 14 patients, ages 1 month to 17 years (9 males and 5 females), with embryonic tumours treated with ifosfamide, alone or combined, at a public tertiary referral hospital. Ifosfamide blood levels ranged from 11.1 to 39.7 μmol/L at 12 hours after the last infusion, while 24-hour levels ranged from 0.7-19.7 μmol/L. The median at 12 hours was 19.5 μmol/L (Q25 14.4-Q75 29.0) and 3.8 μmol/L (Q25 1.5-Q75 9.9) at 24 hours, p<0.001. This method is feasible to determine ifosfamide plasma levels in paediatric patients.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Adolescent
  • Child
  • Child, Preschool
  • Chromatography, High Pressure Liquid / methods*
  • Cyclophosphamide
  • Demography
  • Dried Blood Spot Testing / methods*
  • Female
  • Hematocrit
  • Humans
  • Ifosfamide / blood*
  • Infant
  • Infant, Newborn
  • Male
  • Neoplasms, Germ Cell and Embryonal / blood*
  • Reproducibility of Results
  • Tandem Mass Spectrometry / methods*

Substances

  • Cyclophosphamide
  • Ifosfamide

Grants and funding

The authors thank Consejo Nacional de Ciencia y Tecnología, Fondo Sectorial Salud SSA-2012-179406 (JLCP), and Fondo Federal, Instituto Nacional de Pediatría 068-2013 (LMT). The funders had no role in study design, data collection and analysis, decision to publish or preparation of the manuscript.