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Wang Y.,Shenyang Pharmaceutical University | Wang Y.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Wen J.,Shenyang Pharmaceutical University | Zheng W.,Shenyang Pharmaceutical University | And 6 more authors.
Biomedical Chromatography | Year: 2015

A simple, specific and sensitive ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established and validated for simultaneous determination of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid and geniposide in rat plasma using puerarin as an internal standard (IS). Plasma samples were pretreated by a one-step direct protein precipitation procedure with acetonitrile after acidified using as little as 50μL plasma. Chromatographic separation was performed on an Acquity BEH C18 column (100×2.1mm, 1.7μm) at a flow rate of 0.2mL/min by a gradient elution, using 0.2% acetic acid-methanol as mobile phase. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via electrospray ionization source with negative ion mode. Calibration curves showed good linearity (r>0.995) over wide concentration ranges. The intra- and inter-day precisions were <15%, and the accuracy was within ±8.0%. The validated method was successfully applied to a pharmacokinetic study of the four bioactive components in rats after intravenous administration of Reduning injection. © 2014 John Wiley & Sons, Ltd. Source


Li Y.-J.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Li Y.-J.,Jiangsu Kanion Pharmaceutical Co. | Wang Z.-Z.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Wang Z.-Z.,Jiangsu Kanion Pharmaceutical Co. | And 15 more authors.
Rapid Communications in Mass Spectrometry | Year: 2012

RATIONALE The Direct Analysis in Real Time (DART) ionization source coupled with a quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS) system has the capability to desorb analytes directly from samples from complex Chinese herbal preparations without sample cleanup or chromatographic separation. METHODS In this work, a method based on DART/Q-TOF MS/MS has been developed for rapid determination of geniposide present in 'Re Du Ning Injections', a Chinese herbal preparation. The method has been evaluated for both qualitative and quantitative analysis of geniposide in Re Du Ning Injections. RESULTS Variables including polarity for ion detection, DART gas heater temperature, matrix effect and sample presentation speed were investigated. The quantitative method was validated with respect to linearity, sensitivity, repeatability, precision and accuracy by using both internal and external standards. A comparison of the results obtained using the DART-based method was made with those obtained using a conventional High-Performance Liquid Chromatography/Diode-Array Detector (HPLC/DAD) by analyzing geniposide in four batches of Re Du Ning Injections. CONCLUSIONS The DART/Q-TOF MS/MS-based method provides a rapid, efficient and powerful method to analyze compounds from complex Traditional Chinese Medicines with limited sample preparation thus reducing time and complexity of quality control for those materials. Copyright © 2012 John Wiley & Sons, Ltd. Source


Li J.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Li D.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Hu J.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | Bi Y.,State Key Laboratory of New Technology for Chinese Medicine Pharmaceutical Processes | And 2 more authors.
Biomedical Chromatography | Year: 2015

The study of pharmacokinetics of Ginkgo biloba extracts in Traditional Chinese Medicine was relatively recent. In this study, a simple, quick and sensitive LC-MS/MS analytical method was developed for the determination of ginkgolides A, B, C and bilobalide in rat plasma. The analytes were completely separated from the endogenous compounds on an Agilent Zorbax Eclipse plus C18 column (50mm×3.0mm, 1.8μm) using an isocratic elution. The single-run analysis time was as short as 5.0min. Sample preparation for protein removal was accomplished used a simple methanol precipitation method, after SPE showing a simultaneous extraction and cleanup of extracts allowing for a direct analysis. Extraction recoveries in rat plasma for ginkgolides A, B, C and bilobalide ranged from 75.6% to 89.0%. The calibration curves were determined over the ranges 0.5-20,000ng/mL for ginkgolides A, B, C and bilobalide respectively. The lower limits of quantification (LLOQ) of the analytes were 0.5ng/mL. Inter-day and intra-day precision and accuracy were below 15% and between 85 and 115%, respectively. Finally, the developed method was successfully applied to a pharmacokinetic study following oral administration of the Ginkgo biloba extracts to the male ICR rats. © 2015 John Wiley & Sons, Ltd. Source

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