Highly sensitive liquid chromatography-tandem mass spectrometry method for quantification of a new bone anabolic agent, TAK-778, in human serum

J Pharm Biomed Anal. 2002 Sep 5;30(2):299-305. doi: 10.1016/s0731-7085(02)00269-8.

Abstract

A liquid chromatography-tandem mass spectrometric (LC-MS-MS) method for the highly sensitive determination of a new bone-anabolic agent, TAK-778 in human serum was developed. The internal standard (I.S.) used was deuterated TAK-778. TAK-778 and I.S. were extracted from serum samples with diethyl ether at neutral pH. A turbo ion spray interface was used as the ion source of LC-MS-MS, and the analysis was performed in the selected reaction monitoring mode. The lower limit of quantification was 0.02 ng/ml when 0.4 ml of serum was used, and the standard curve was linear in the range of 0.02-10 ng/ml. The method was precise; the intra- and inter-day precision of the method was not more than 17.9%. The accuracy of the method was good with the deviations between added and calculated concentration of TAK-778 being typically within 9.0%.

MeSH terms

  • Anabolic Agents / blood*
  • Anabolic Agents / chemistry
  • Benzothiepins / blood*
  • Benzothiepins / chemistry
  • Chromatography, High Pressure Liquid / methods
  • Chromatography, High Pressure Liquid / statistics & numerical data
  • Humans
  • Mass Spectrometry / methods
  • Mass Spectrometry / statistics & numerical data

Substances

  • Anabolic Agents
  • Benzothiepins
  • TAK 778