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HPLC-MS Method (HPLC-M + method)
Selected AbstractsDetermination of glycyrrhetic acid in human plasma by HPLC-MS method and investigation of its pharmacokineticsJOURNAL OF CLINICAL PHARMACY & THERAPEUTICS, Issue 3 2008W.-J. Zhao PhD Summary Objective:, To develop a high performance liquid chromatography mass spectrometry (HPLC-MS) method for the determination of the glycyrrhetic acid (GA) in human plasma and for the investigation of its pharmacokinetics after the oral administration of 150 mg diammonium glycyrrhizinate test and reference capsule formulations. Methods:, The GA in plasma was extracted with ethyl acetate, separated on a C18 column with a mobile phase of methanol (5 mmol/L ammonium acetate),water (85 : 15, V/V) and analysed using a MS detector. Ursolic acid (UA) was used as internal standard. The target ions were m/z 469·5 for GA and m/z 455·6 for UA, the fragment voltages were 200 V and 100 V for GA and UA respectively. Results:, The calibration curve was linear over the range of 0·5,200 ng/mL (r = 0·9974). The limit of quantification for GA in plasma was 0·5 ng/mL, the recovery was 76·0,80·0%, and the inter- and intra-day relative standard deviations (RSD) were <12%. The pharmacokinetic parameters of GA after a single dose of 150 mg diammonium glycyrrhizinate test and reference were as follows: the half life (t1/2) 9·65 ± 3·54 h and 9·46 ± 2·85 h, the time to peak concentration (Tmax) 10·95 ± 1·32 h and 11·00 ± 1·30 h, the peak concentration (Cmax) 95·57 ± 43·06 ng/mL and 103·89 ± 49·24 ng/mL; the area under time-concentration curve (AUC0,48 and AUC0,,) 1281·84 ± 527·11 ng·h/mL and 1367·74 ± 563·27 ng·h/mL, 1314·32 ± 566·40 ng·h/mL and 1396·97 ± 630·06 ng·h/mL. The relative bioavailability of diammonium glycyrrhizinate capsule was 98·88 ± 12·98%. Conclusion:, The assay was sensitive, accurate and convenient, and can be used for the determination of GA in human plasma. Comparison of the bioavailability and pharmacokinetic profile of GA indicated that the test and reference capsules were bioequivalent. [source] A simple HPLC-MS method for the quantitative determination of the composition of bacterial medium chain-length polyhydroxyalkanoatesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 10 2008Andreas Grubelnik Abstract Bacterial poly(hydroxyalkanoates) (PHAs) vary in the composition of their monomeric units. Besides saturated side-chains, unsaturated ones can also be found. The latter leads to unwanted by-products (THF ester, secondary alcohols) during acidic cleavage of the polymer backbone in the conventional analytical assays. To prevent these problems, we developed a new method for the reductive depolymerization of medium chain-length PHAs, leading to monomeric diols that can be separated and quantified by HPLC/MS. Reduction is performed at room temperature with lithium aluminum hydride within 5,15 min. The new method is faster and simpler than the previous ones and is quantitative. The results are consistent with the ones obtained by quantitative 1H NMR. [source] A combined HPLC-UV and HPLC-MS method for the identification of lignans and its application to the lignans of Linum usitatissimum L. and L. bienne Mill.,PHYTOCHEMICAL ANALYSIS, Issue 5 2006Thomas J. Schmidt Abstract A combined HPLC-UV/PAD and HPLC-ESI/MS method allowing the fast detection and identification/structural characterisation of lignans of different structural subclasses is described. Twenty-four lignans of different skeletal types were analysed and the combined information derived from their UV and ESI/MS spectra led to the identification of group characteristics that can be used to establish the structure of unknown lignans in plant samples. This method was successfully applied to the identification of lignans in crude extracts of Linum usitatissimum L. and L. bienne Mill. Copyright © 2006 John Wiley & Sons, Ltd. [source] Determination and toxicokinetics comparison of ketamine and S(+)-ketamine in dog plasma by HPLC-MS methodBIOMEDICAL CHROMATOGRAPHY, Issue 3 2010Yu-xin Sheng Abstract ;A simple and reproducible method was developed for the quantification of ketamine and S(+)-ketamine in dog plasma using a high-performance liquid chromatography system coupled to a positive ion electrospray mass spectrometric analysis. Solid-phase extraction was used for extracting analytes from dog plasma samples. The analytes were separated on a Zorbax SB C18 column (100 × 2.1 mm, 3.5 ,m) with acetonitrile,formate buffer (10 mM ammonium formate and 0.3% formic acid) (17 : 83, v/v) as mobile phase at a flow-rate of 0.2 mL/min. Detection was operated under selected ion monitoring mode. [M + H]+ at m/z 238 for ketamine and S(+)-ketamine and [M + H]+ at m/z 180 for phenacetin (internal standard) were selected as detecting ions, respectively. The method was linear in the concentration range 51.6,2580 ng/mL. The intra- and inter-day precisions (RSD %) were within 11.3% and the assay accuracies ranged from 80.0 to 101.4%. Their average recoveries were greater than 91.1% at all test concentrations. The analytes were proved to be stable during all sample storage, preparation and analysis procedures. The method was successfully applied to the toxicokinetics study and comparison of ketamine and S (+)-ketamine following intravenous administration to dogs. Copyright © 2009 John Wiley & Sons, Ltd. [source] An HPLC-MS method for simultaneous estimation of ,,, -arteether and its metabolite dihydroartemisinin, in rat plasma for application to pharmacokinetic studyBIOMEDICAL CHROMATOGRAPHY, Issue 7 2003M. Rajanikanth Abstract This manuscript reports, the development and validation of a sensitive and selective assay method for simultaneous determination of ,,, -arteether and its metabolite dihydroartemisinin (DHA) in rat plasma by liquid chromatography,mass spectrometry. Chromatographic separations were achieved by gradient elution of the analytes with an initial composition of methanol,potassium acetate buffer (pH 4; 73:27, v/v) to 100% methanol in 3 min and maintained for 5 min on a Spheri-10, RP18 (100 × 4.6 mm i.d.) column following an RP18 (30 × 4.6 mm i.d.) guard column. The total ef,uent from the column was split so that one-tenth was injected into the electrospray LC/MS interface. ESI-MS analysis was performed using a Micromass Quattro II Triple Quadrupole Mass Spectrometer equipped with an electrospray source. The MS analysis was carried out at cone voltage of 22 V with a scan range of 200,500 Da. The analytes were quanti,ed from the [M+ K]+ ion chromatograms of ,,, -arteether at m/z 352, DHA at m/z 323, artemisinin at m/z 321 and propyl ether analogue of arteether at m/z 365. Liquid,liquid extractions with a combination of n -hexane and hexane,ethyl acetate (8:2) were used to isolate ,,, -arteether and DHA from rat plasma. The method was validated and gave good accuracy and precision for the studied domain. Linearity in serum was observed over the range 4.375,70 ng/mL for a -arteether and 10,160 ng/mL for , -arteether and DHA. Percentage bias (accuracy) and within- and between-assay precision were well within the acceptable range. This method was applied to study the pharmacokinetics following oral administration of ,,, -arteether (30 mg/kg) in rats. Copyright © 2003 John Wiley & Sons, Ltd. [source] | ||||||||||