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Simultaneous Determination of Salidroside and Its Aglycone Metabolite p-Tyrosol in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry
Alkali Soil Natural Environmental Science Center, Northeast Forestry University/Key Laboratory of Saline-alkali Vegetation Ecology Restoration in Oil Field, Ministry of Education, Harbin 150040, China
College of Life Sciences, Heilongjiang University, Harbin 150080, China
These authors contributed equally to this work.
* Authors to whom correspondence should be addressed.
Received: 17 January 2012; in revised form: 3 April 2012 / Accepted: 13 April 2012 / Published: 23 April 2012
Abstract: Salidroside and its aglycone p-tyrosol are two major phenols in the genus Rhodiola and have been confirmed to possess various pharmacological properties. In our present study, p-tyrosol was identified as the deglycosylation metabolite of salidroside after intravenous (i.v.) administration to rats at a dose of 50 mg/kg, but was not detectable after intragastric gavage (i.g.) administration through HPLC-photodiode array detection (PDA) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Next, an accurate and precise LC-MS/MS method was developed to quantitatively determine salidroside and p-tyrosol in rat plasma samples. Samples were analyzed by LC-MS/MS on a reverse-phase xTerra MS C18 column which was equilibrated and eluted with an isocratic mixture of acetonitrile-water (1:9, v/v) at a flow rate of 0.3 mL/min. The analytes were monitored by multiple reaction monitoring (MRM) under the negative electrospray ionization mode. The precursor/product transitions (m/z) were 299.0→118.8 for salidroside, 137.0→118.9 for p-tyrosol and 150.1→106.9 for the internal standard (IS), paracetamol, respectively. The calibration curve was linear over the concentration ranges of 50–2,000 ng/mL for salidroside and 20–200 ng/mL for p-tyrosol. The inter- and intra-day accuracy and precision were within ±15%. The method has been successfully applied to the pharmacokinetic study and the oral bioavailability was calculated.
Keywords: salidroside; p-tyrosol; metabolite; LC-MS/MS; pharmacokinetics
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Guo, N.; Hu, Z.; Fan, X.; Zheng, J.; Zhang, D.; Xu, T.; Yu, T.; Wang, Y.; Li, H. Simultaneous Determination of Salidroside and Its Aglycone Metabolite p-Tyrosol in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry. Molecules 2012, 17, 4733-4754.
Guo N, Hu Z, Fan X, Zheng J, Zhang D, Xu T, Yu T, Wang Y, Li H. Simultaneous Determination of Salidroside and Its Aglycone Metabolite p-Tyrosol in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry. Molecules. 2012; 17(4):4733-4754.
Guo, Na; Hu, Zhiwei; Fan, Xiaoxu; Zheng, Jian; Zhang, Dehui; Xu, Tao; Yu, Tao; Wang, Yang; Li, Haiying. 2012. "Simultaneous Determination of Salidroside and Its Aglycone Metabolite p-Tyrosol in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry." Molecules 17, no. 4: 4733-4754.