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  • Title: Simultaneous determination of SYL-1119 and SYL-1119-P in rat plasma using HPLC coupled with tandem mass spectrometry.
    Author: Yang S, Hu J, Li Y.
    Journal: J Chromatogr B Analyt Technol Biomed Life Sci; 2014 Jan 15; 945-946():193-8. PubMed ID: 24355213.
    Abstract:
    SYL-1119 is a sphingosine-1-phosphate receptor 1 modulator for the treatment of autoimmune disease with better selectivity, while SYL-1119-P is its active phosphate. A sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of SYL-1119 and SYL-1119-P in rat plasma. SYL-1110, an analogue of SYL-1119, was used as the internal standard. Plasma samples were prepared by protein precipitation using acetonitrile. The analytes and internal standard were separated on a Zorbax SB-C18 column (3.5μm, 100mm×2.1mm) with a gradient mobile phase consisting of methanol and water containing 0.1% formic acid at a flow rate of 0.2ml/min with an operating temperature of 20°C. The detection was performed on a triple quadrupole tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode of the transitions at m/z 364→259 for SYL-1119, m/z 444→259 for SYL-1119-P, and m/z 378→273 for the IS. Calibration curves were linear in the range of 0.2-50ng/ml for SYL-1119 and 10-1000ng/ml for SYL-1119-P. The lower limit of quantification (LLOQ) was 0.2ng/ml for SYL-1119 and 10ng/ml for SYL-1119-P. The intra- and inter-day precisions were 5.4-12.8% for two analytes with accuracies within ±10%. The recoveries for two compounds were 91.3-104.5%. The analytes were proved to be stable during all sample storage, preparation, and analytic procedures. The method was successfully applied to the pharmacokinetic study of SYL-1119 and SYL-1119-P in rats after oral administration of SYL-1119.
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