-
[show abstract]
[hide abstract]
ABSTRACT: Acanthopanax sessiliflorus (Rupr. et Maxim.) Seem. is a shrub mainly present in China, Japan and Korea, the root bark of which is considered as one of the sources of Wujiapi and widely used for its various pharmacological effects.
A selective and sensitive UPLC-MS/MS method was developed and validated for the determination and pharmacokinetic study of asarinin, sesamin, helioxanthin and savinin in rat plasma.
Sample preparation involved a liquid-liquid extraction of the analytes with methyl tert-butyl ether (MTBE). LC separation was achieved on a UPLC C(18) column at 30°C with a mobile phase consisting of methanol-2 mM ammonium acetate (68:32, v/v). The detection was accomplished by multiple-reaction monitoring (MRM) scanning with electrospray ionization (ESI) source operating in the positive ionization mode. The optimized mass transition ion-pairs (m/z) monitored for asarinin, sesamin, helioxanthin, savinin and IS were 372.2/233.0, 372.2/233.0, 349.1/319.0, 352.9/334.9 and 180.0/109.7, respectively.
The current LC-MS/MS assay was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery and stability and was suitable for pharmacokinetic studies of the four lignans after oral administration of Acanthopanax sessiliflorus extract. The time to reach the maximum plasma concentration (T(max)) was 2.50±0.15 h for asarinin, 1.94±0.28 for sesamin, 2.22±0.48 h for helioxanthin and 2.83±0.29 h for savinin. The elimination half-time (t(1/2)) of asarinin, sesamin, helioxanthin and savinin was 6.08±1.10, 11.69±0.50, 7.16±0.52 and 6.26±0.57 h, respectively.
This paper described a simple, sensitive and validated UPLC-MS/MS method for simultaneous determination of four lignans in rat plasma after oral administration of Acanthopanax sessiliflorus extract, and investigated on their pharmacokinetic studies as well.
Journal of ethnopharmacology 04/2012; 141(3):957-63. · 2.32 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: A UPLC-MS/MS method was developed for the simultaneous determination of paeoniflorin, naringin, naringenin and glycyrrhetinic acid in rat plasma. A Waters BEH C(18) column was used with a gradient mobile phase system of methanol-water containing 2 mM ammonium acetate. The analysis was performed on a positive ionization electrospray mass spectrometer via multiple reaction monitoring (MRM). One-step protein precipitation with acetonitrile was used to extract the analytes from plasma. The limits of quantification were 9.800 ng/ml for paeoniflorin, 5.100 ng/ml for naringin, 5.200 ng/ml for naringenin and 10.60 ng/ml for glycyrrhetinic acid, respectively. The intra- and inter-day precision (relative standard deviation, RSD) ranged 4.9-12% and 2.8-13%, respectively. The accuracy (relative error, RE) was from -7.3% to 7.5% at all quality control (QC) levels. The validated method was applied to a pharmacokinetic study in rats after oral administration of Si-Ni-San decoction.
Journal of pharmaceutical and biomedical analysis 03/2012; 66:271-7. · 2.45 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: A rapid and selective ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for simultaneous determination of three bioactive coumarins of Toddalia asiatica extract including pimpinellin, isopimpinellin and phellopterin in rat plasma for the first time. Phenacetin was used as the internal standard (IS). Plasma samples were extracted by liquid-liquid extraction with methyl tert-butyl ether. The chromatographic separation was carried out on an ACQUITY UPLC™ BEH C₁₈ column with an isocratic mobile phase consisting of methanol-5 mmol/L ammonium acetate (65:35, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) via electrospray ionization (ESI) source with positive ionization mode. The method was linear for all analytes over investigated range with all correlation coefficients greater than 0.9942. The lower limits of quantification (LLOQ) were 25.0 ng/mL for pimpinellin, 10.0 ng/mL for isopimpinellin and 5.00 ng/mL for phellopterin. The intra- and inter-day precision (RSD%) was within 12% and the accuracy (RE%) ranged from -2.3% to 5.5%. The rapid and sensitive method was fully validated and successfully applied to the pharmacokinetic study of pimpinellin, isopimpinellin and phellopterin in rats following oral administration of Toddalia asiatica extract.
Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 02/2012; 891-892:102-8. · 2.78 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: A simple and reliable high-performance liquid chromatographic (HPLC) method has been developed for the determination of nodakenin in rat plasma. The concentration of nodakenin was determined in plasma samples after deproteinization with methanol using hesperidin as internal standard. HPLC analysis was performed on a Diamonsil C(18) analytical column using acetonitrile-water (25:75, v/v) as the mobile phase and a UV detection at 330 nm. This method was validated in terms of recovery, linearity, accuracy and precision (intra- and inter-day variation). The extraction recoveries were 91.3 ± 10, 87.8 ± 4.8 and 92.6 ± 5.1 at concentrations of 0.500, 5.00 and 40.0 μg/mL, respectively. The standard curve for nodakenin was linear (r(2) ≥ 0.99) over the concentration range 0.250-50.0 μg/mL with a lower limit of quantification of 0.250 μg/mL. The intra- and inter-day precision (relative standard deviation, RSD) values were not higher than 12% and the accuracy (relative error, RE) was within ± 5.8% at three quality control levels. The validated method was successfully applied for the evaluation of the pharmacokinetics of nodakenin in rats after oral administration of Rhizoma et Radix Notopterygii decoction and nodakenin solution.
Biomedical Chromatography 12/2010; 25(10):1076-80. · 1.97 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: To identify five constituents in the aqueous extract of Isatis indigotica Fort.
After separation of the aqueous extract of Isatis indigotica Fort. by HPLC, the eluates of five peaks were collected separatively and analysed by MS2. UV spectra and MS2 were compared with those of reference standards of cytidine, uridine, guanosine xanthine and hypoxanthine.
Each HPLC elute of the aqueous extract had same retention time, UV spectra and fragment pattern in the MS2 spectrum as the corresponding standards.
Five constituents of the aqueous extract of Isatis indigotica Fort. are identified as cytidine, hypoxanthine, uridine, xanthine and guanosine.
Zhong yao cai = Zhongyaocai = Journal of Chinese medicinal materials 10/2005; 28(9):772-4.
-
[show abstract]
[hide abstract]
ABSTRACT: Binary chromatographic profiling was employed in fingerprint analysis of Flos Lonicerae japonicae, the flower bud of Lonicera japonica Thunb. Standardized procedures were used to develop the profiling for both aqueous and ethanolic extracts. Other species in the previous Chinese Pharmacopoeia and some in folk remedy were successfully differentiated from L. japonica Thunb. by hierarchiral cluster analysis of the chromatographic profiles. Correlation analysis showed that six chromatographic peaks in ethanolic extract were positively correlated with in vitro bacteriostasis activity. Two standard fingerprints were developed with 10 genuine samples of L. japonica Thunb. Similarity analysis with a limited number of samples showed a fair consistence in the chromatographic profiling of L. japonica Thunb. from various sources and two harvests, and significant differences from other species. Combination use of the two fingerprints demonstrated confirmative identification and quality assessment of Flos Lonicerae japonicae.
Biomedical Chromatography 20(6-7):634-41. · 1.97 Impact Factor
