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Chem. J. Chinese Universities ›› 2009, Vol. 30 ›› Issue (8): 1528.

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Liquid Chromatography-Tandem Mass Spectrometric Assay for the Determination of CTN986 and Its Deglycosylation Products in the Rat Brain Dialysate

GUO Ji-Fen1, ZHANG Shao-Dong2, MENG Fan-Hua1, ZHAO Yi-Min1*   

  1. 1. Institute of Pharmacology and Toxicology, Academy of Military Medical Science, Beijing 100850, China;
    2. Beijing Neurosurgical Institute, Beijing 100050, China
  • Received:2008-12-30 Online:2009-08-10 Published:2009-08-10
  • Contact: ZHAO Yi-Min. E-mail: zhaoym@nic.bmi.ac.cn
  • Supported by:

    国家自然科学基金(批准号: 30672508)和北京市自然科学基金(批准号: 7072061)资助.

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Abstract:

An HPLC-MS/MS method was developed for the determination of CTN986 and its two deglycosylation products, rutin and hirsutin, in the rat brain dialysate. The dialysate samples were analyzed by offline liquid chromatography-tandem mass spectrometry. The separation was performed using a Zorbax C8 column with an isocratic mobile phase consisted of methanol/isopropanol/water/formic acid(20∶10∶70∶0.1, volume ratio). An API 3000 tandem mass spectrometer equipped with electrospray ionization source was used as detector and was operated under the positive ion mode. Multiple reactions monitoring(MRM) mode was used to quantify three analytes. Calibration was performed by external standardization and regression curves were constructed ranging from 2 to 500 ng/mL for each compound. The intra- and inter-day precision values were below 15% and accuracy was between -4% and 13% for all quality control samples. As a result, the procedure proved to be very suitable for routine analysis. This quantitation method was applied to the pharmacokinetic study of CTN986 in the brain dialysate samples from rats following oral administration.

Key words: CTN986; Liquid chromatography-tandem mass spectrometry; Microdialysis

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