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ABSTRACT: Chiisanogenin existing in many Acanthopanax species has been reported to possess anti-inflammatory, antibacterial and antiplatelet aggregatory activities.
To develop and validate a rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry method for the determination of chiisanogenin in rat plasma and to investigate its pharmacokinetics after oral administration of chiisanogenin or the extract of Acanthopanax sessiliflorus fruits.
The sample pretreatment involved a one-step extraction of 0.2 mL plasma with diethyl ether. Acetaminophen was used as the internal standard. The separation was carried out on an ACQUITY UPLC™ BEH C₁₈ column with a mobile phase of acetonitrile-5 mM ammonium acetate (90:10, v/v) at a flow rate of 0.2 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source.
A high sample throughput was achieved with an analysis time of 1.1 min per sample. The calibration curve was linear (r² ≥ 0.99) over the concentration range of 5-500 ng/mL with a lower limit of quantification (LLOQ) of 5 ng/mL. The intra-day and inter-day precision (relative standard deviation, R.S.D.) values were below 11% and the accuracy (relative error, R.E.) was within 8% at all three quality control (QC) levels.
The method was successfully applied to the pharmacokinetic study of chiisanogenin in rat after oral administration of chiisanogenin and the extract of Acanthopanax sessiliflorus fruits. Other constituents in the extract affected the pharmacokinetic behavior of chiisanogenin.
Phytochemical Analysis 11/2010; 22(3):225-9. · 2.63 Impact Factor
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ABSTRACT: To isolate and elucidate the chemical constituents of the fruits of Acanthopanax sessiliflorus.
Isolation and purification were carried out on the column chromatography of silica gel and Sephadex LH-20. Their structures were elucidated on basis of physicochemical properties and spectral data.
Nine compounds were isolated and identified as oleanolic acid-3-O-6'-O-methyl-beta-D-glucuronopyranoside (1), 22-alpha-hydroxychiisanogenin (2), oleanolic acid-3-O-beta-D-glucuronopyranoside (3), oleanolic acid-3-O-beta-D-glucopyranoside (4), oleanolic acid (5), chiisanogenin (6), (-)-sesamin (7), daucosterol (8), beta-sitosterol (9).
Compound 1 is obtained from the genus Acanthopanax genus for the first time. Compounds 2-5 are isolated from this plant for the first time.
Zhongguo Zhong yao za zhi = Zhongguo zhongyao zazhi = China journal of Chinese materia medica 04/2009; 34(6):715-7.
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ABSTRACT: One new triterpenoid saponin and two lupane-derived triterpenes were isolated from Acanthopanax sessiliflorus fruits. The structures of the two new compounds were elucidated as 3- O-[(alpha- L-arabinopyranosyl)-(1 --> 2)]-[ beta- D-glucuronopyranosyl-6- O-methyl ester]-olean-12-ene-28-olic acid (1) and (1 R,11 alpha,22 alpha)-1,4-epoxy-11,22-hydroxy-3,4-secolupane-20(30)-ene-3,28-dioic acid (3) on the basis of spectral analysis, including MS, (1)H-NMR, (13)C-NMR, DEPT, HMBC, HMQC and NOESY. The structure of the other new natural product was elucidated as (1 R,11 alpha)-1,4-epoxy-11-hydroxy-3,4-secolupane-20(30)-ene-3,28-dioic acid (2). All these compounds showed antiplatelet aggregation activity on ADP-induced platelet aggregation.
Planta Medica 03/2009; 75(6):656-9. · 2.15 Impact Factor
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ABSTRACT: A method was developed for the quantitative determination of protocatechuic acid in rat plasma by high performance liquid chromatography (HPLC). With added p-hydroxybenzoic acid as internal standard, the plasma samples were extracted with a solvent mixture of methanol and acetonitrile ( 1: 5, v/v). The analyte was determined by HPLC with a Diamondsil C18 column and a mobile phase of acetonitrile-water (adjusted to pH 2.5 with H3PO4, 9: 91, v/v) at a flow rate of 1. 2 mL/min. The UV detection wavelength was 260 nm. The assay exhibited a good linearity in the concentration range from 0. 050 to 3. 20 mg/L with a correlation coefficient of 0. 997 8. The limit of quantification was 0. 050 mg/L. The relative standard deviations of intra-day and inter-day determination were both less than 7. 0% and the accuracy ranged from - 1. 4% to 2. 6%. The extraction recoveries of protocatechuic acid from rat plasma samples at three concentration levels were 83. 4%, 87. 3%, and 91. 1%, respectively. The developed method was applied to a pharmacokinetic study. The main pharmacokinetic parameters in rats after a single oral dose of 10 mL/kg body weight were as follows: Cmax of (3. 16 +0. 03) microg/mL, tmax of (0. 50 +/- 0. 00) h, AU0-->t of (39. 9 +/- 5. 9) microg x mL(-1) x h, AUC-->infinity of (54. 8 +/- 8. 1) microg x mL(-1) x h and t1/2 of (3. 87 +/- 0. 25) h. The method was proved to be simple, sensitive and accurate, thus suitable for the pharmacokinetic study of protocatechuic acid in rat plasma.
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 03/2007; 25(2):207-10.
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ABSTRACT: A sensitive, specific method has been developed for simultaneous determination of neoeriocitrin and naringin in rat plasma using liquid chromatography-tandem mass spectrometry. With hesperidin as the internal standard, plasma samples were prepared by protein precipitation with methanol. Analysis was carried out on an ACQUITY UPLC BEH C(18) column using acetonitrile-water (20:80, v/v) as the mobile phase. Detection was performed by means of electrospray ionization mass spectrometry in negative ion mode with multiple reaction monitoring. Linear calibration curves of neoeriocitrin and naringin were obtained over the concentration ranges of 15.0-960 ng/mL and 12.0-1200 ng/mL, respectively. The intra- and inter-day precisions were within 9.7% and 7.6% for neoeriocitrin and 7.8% and 12.9% for naringin. The accuracy was from -4.3% to 0.43% for neoeriocitrin and from -3.8% to 3.0% for naringin. The validated method was successfully applied to the pharmacokinetic study of neoeriocitrin and naringin in rats after oral administration of a Chinese compound formulation, gushudan.
Journal of chromatographic science 48(5):342-7. · 0.88 Impact Factor
