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Determination of oleanolic acid in human plasma and study of its pharmacokinetics in Chinese healthy male volunteers by HPLC tandem mass spectrometry by Min Song; Tai-jun Hang; Ying Wang; Li Jiang; Xiao-luan Wu; Zhengxing Zhang; Jianping Shen; Yindi Zhang is a Chemistry article available to read on EtoBox.
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A highly selective and sensitive HPLC-ESI-MS-MS method was developed for the determination of oleanolic acid in human plasma. The oleanolic acid and glycyrrhetinic acid (internal standard) were recovered from plasma with ethyl acetate liquid-liquid extraction. The organic extracts were dried under a stream of warm nitrogen, reconstituted in mobile phase and injected into a Zorbax-Extend ODS analytical column (150 mm × 4.6 mm i.d., 5 m), with the mobile phase consisting of methanol-ammonium acetate (32.5 mM) (85:15, v/v) pumped at a flow rate of 1.0 ml/min, and 30% of the eluent was split into a MS system with electrospray ionization tandem mass (ESI-MS-MS) detection in negative ion mode. The tandem mass detection was performed on a Finnigan Surveyor LC-TSQ Quantum Ultra AM tandem mass spectrometer operated in selected reaction monitoring mode. The parent to product ion combinations of m/z 455.4 → 455.4 and 469.3 → 425.2 at 38 V 1.5 mTorr Ar CID were used to quantify oleanolic acid and glycyrrhetinic acid, respectively. The assay was validated in the concentration range of 0.02-30.0 ng/ml for oleacolic acid when 0.5 ml of plasma was processed. The precision of the assay (expressed a
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- Author
- Min Song; Tai-jun Hang; Ying Wang; Li Jiang; Xiao-luan Wu; Zhengxing Zhang; Jianping Shen; Yindi Zhang
- Publisher
- Elsevier Science; Elsevier ; Elsevier BV (ISSN 0731-7085)
- Published
- 2006
- Language
- EN
- Field
- Chemistry (Physical Sciences)