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LC-MS/MS determination of helicid in human plasma and its application in pharmacokinetic studies.

Abstract
Helicid is a traditional Chinese medicine used to treat headache and insomnia with definite effects. To facilitate pharmacokinetic studies of helicid in man, a sensitive and specific LC-MS/MS method for the quantitative detection of helicid in human plasma was developed and validated. The method involved the addition of bergeninum as the internal standard (IS), protein precipitation, HPLC separation, and quantification by MS/MS system using negative electrospray ionization in the multiple reaction monitoring mode (MRM). The precursor→product ion transitions were monitored at m/z 282.8→120.9 for helicid and m/z 326.9→192.2 for the IS, respectively. The lower limit of quantification (LLOQ) was 0.2 μg/L. The calibration curves for helicid was linear over a concentration range of 0.2-20 μg/L. The intra- and inter-batch analyses of QC samples at 0.4, 2, 20 μg/L indicated good precision (%R.S.D. between 2.69 and 5.47%) and accuracy (between 96.15 and 105.05%). The helicid was stable in human plasma stored at room temperature for at least 24h, 4°C for at least 24h, -20°C for at least 1 month, and for routine three freeze-thaw cycles. This accurate and specific assay provides a useful method for evaluating the pharmacokinetic profile of helicid in humans.
AuthorsHaitang Xie, Yuanwei Jia, Zhirong Tan, Wei Zhang, Rao Chen, Hua Sun, Jie Shen, Honghao Zhou
JournalJournal of chromatography. B, Analytical technologies in the biomedical and life sciences (J Chromatogr B Analyt Technol Biomed Life Sci) Vol. 879 Issue 30 Pg. 3607-11 (Nov 15 2011) ISSN: 1873-376X [Electronic] Netherlands
PMID22024391 (Publication Type: Journal Article, Research Support, Non-U.S. Gov't)
CopyrightCopyright © 2011 Elsevier B.V. All rights reserved.
Chemical References
  • Benzaldehydes
  • Drugs, Chinese Herbal
  • helicide
Topics
  • Benzaldehydes (blood, pharmacokinetics)
  • Chromatography, Liquid (methods)
  • Drug Stability
  • Drugs, Chinese Herbal
  • Humans
  • Linear Models
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry (methods)

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