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ABSTRACT: In this study, a simple and sensitive LC/MS/MS method was developed and validated for the determination of arctigenin in rat plasma. The MS detection was performed using multiple reaction monitoring at the transitions of m/z 373.2 → 137.3 for arctigenin and m/z 187.1 → 131.0 for psoralen (internal standard) with a Turbo IonSpray electrospray in positive mode. The calibration curves fitted a good linear relationship over the concentration range of 0.2-500 ng/mL. It was found that arctigenin is not stable enough at both room temperature and -80 °C unless mixed with methanol before storage. The validated LC/MS/MS method was successfully applied for the pharmacokinetic study of arctigenin in rats. After intravenous injection of 0.3 mg/kg arctigenin injection to rats, the maximum concentration, half-life and area under the concentration-time curve were 323 ± 65.2 ng/mL, 0.830 ± 0.166 and 81.0 ± 22.1 h ng/mL, respectively. Copyright © 2013 John Wiley & Sons, Ltd.
Biomedical Chromatography 05/2013; · 1.97 Impact Factor
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ABSTRACT: 5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it
is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore,
a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the
determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed
on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium
formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector
at 265 nm. The calibration curve was linear over the concentration range of 5–500 ng/mL and the correlation coefficient was
not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively,
and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible
conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies
of 5-FU in human.
Keywords5-fluorouracil(5-FU)-high-performance liquid chromatography (HPLC)-human plasma
Transactions of Tianjin University 04/2012; 16(3):167-173.
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ABSTRACT: We developed a rapid, simple and sensitive LC/MS/MS method for the simultaneous quantitation of tegafur (FT) and gimeracil (CDHP) in human plasma with a concentration range of 20-5000 and 2-500 ng/mL, respectively. Methanol was chosen as a precipitation agent for sample preparation. Chromatographic separation was performed on an inertsil ODS-3 C18 column using 1.0% formic acid in water and methanol (80/20, v/v) at a flow rate of 0.3 mL/min. The MS detection was operated with selected reaction monitoring (SRM) in the positive-ion mode. The matrix effect ranged from -8.9 to 7.8% for all analytes. The intra- and inter-day precisions were less than 8.6 and 9.5%, and the accuracy was within +/-7.5% for all analytes, respectively. The mean recoveries were 76.5 +/- 5.2 and 78.3 +/- 5.9% for FT and CDHP, respectively. The analytes were stable under all possible conditions of storing and handling for each compound.
Analytical Sciences 10/2009; 25(10):1211-5. · 1.25 Impact Factor
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ABSTRACT: A sensitive, rapid and specific liquid chromatography/tandem mass spectrometry (LC/MS/MS) assay has been established for the quantitation of catalpol in rat plasma. Plasma samples were treated by precipitating protein with methanol and were chromatographed by a Diamonsil C(18) column (150 mm x 4.6 mm I.D., 5 microm) with the mobile phase consisting of methanol and 10 mM ammonium formate (30:70, v/v). The selected reaction monitoring (SRM) transitions were performed at m/z 380.1-->183.0 for catalpol and m/z 364.3-->167.0 for aucubin (IS) in the positive ion mode with electrospray ionization (ESI) source. Calibration curve was linear over the concentration range of 10-20,000 ng/mL. The mean recovery was 76.5+/-5.2% and the matrix effect ranged from -5.1 to 13.0%. The intra- and inter-day precisions were less than 6.3 and 14.6%, respectively, and the accuracy was within +/-5.6%. Catalpol was stable in possible conditions of storing and handling. The validated method has been successfully applied to determine the plasma concentration of catalpol for a pharmacokinetic study of catalpol after oral administration of 50 mg/kg to rats.
Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 09/2009; 877(29):3589-94. · 2.78 Impact Factor
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ABSTRACT: ZT-1 is a novel acetylcholinesterase (AChE) inhibitor. It is rapidly transformed to Huperzine A (Hup A) in vitro. A simple and rapid HPLC-UV method for the simultaneous determination of ZT-1 and its metabolite Hup A in plasma is described. The chromatographic separations were achieved on a C(18) ODS column (250 mm x 4.6 mm ID) using methanol-1 mmol/L ammonium acetate (70:30,v/v) as mobile phase. The flow rate was 0.7 mL/min, the detection wavelength was 313 nm and the column temperature was kept at 35 degrees C. Plasma samples were prepared as rapidly as possible and extracted immediately with 5 mL of chloroform:iso-propyl alcohol mixture (v/v, 9:1). The retention times of ZT-1 and Huperzine A (Hup A) were 18.7 and 14.4 min, respectively. The mean absolute recoveries of two analytes were >90%. Quantification limits were all 0.02 nmol/mL for ZT-1 and Hup A. This analytical method was reliable and convenient procedure that meets the criteria for the pharmacokinetic evaluation of ZT-1 on experimental animals.
Journal of Chromatography B 01/2006; 830(1):120-5. · 2.89 Impact Factor
