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Cui Y.,Shenyang Pharmaceutical University | Cui Y.,Shandong Luoxin Pharmaceutical Co. | Ma N.,Liaoning Academy of Chinese Medicine | Li X.,Shenyang Pharmaceutical University | And 6 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2014

A new, sensitive and efficient ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method has been developed and validated for simultaneous quantification of cefazedone and etimicin in beagle dog plasma. After addition of the internal standard (IS) metronidazole, plasma samples were treated by protein precipitation procedure, and then separated on a Venusil MP C18 column (100mm×2.1mm, 3.0μm) (Venusil, China) using gradient elution with the mobile phase consisting of 0.01% heptafluorobutyric acid (HFBA) in acetonitrile and 0.01% HFBA in water at a flow rate of 0.4mLmin-1. The detection of the analytes was performed on 4000Q UFLC-MS/MS system with turbo ion spray source in the positive ion and multiple reaction-monitoring (MRM) mode. The linear range was 1.0-200μgmL-1 for cefazedone and 0.5-100μgmL-1 for etimicin, with lower limits of quantification of 1.0 and 0.5μgmL-1, respectively. Intra-day and inter-day precisions were within 7.2% and 4.3%, respectively for both analytes, and the accuracy (relative error, RE, %) was less than 10.7% and 12.7%, respectively. The mean absolute extraction recoveries of analytes and IS from beagle dog plasma were all more than 73.22%. The validated method was successfully applied to the pharmacokinetic study of cefazedone and etimicin in beagle dog after intravenous administration of cefazedone injection combined with etimicin injection and the two single injections alone, respectively. The results indicated there were not obvious differences between the pharmacokinetic behaviors between the combined group and either of the single groups. © 2014 Elsevier B.V.

Zhang Y.,Shenyang Pharmaceutical University | Zhang Y.,Liaoning Academy of Chinese Medicine | Diao Y.-P.,Liaoning University of Traditional Chinese Medicine | You X.-M.,Liaoning Academy of Chinese Medicine | And 5 more authors.
Journal of Medicinal Plants Research | Year: 2010

To control the quality of Zaoren-anshen granule (ZRG), a simple, reliable and reproducible method of High-Performance Liquid Chromatography equipped with Photodiode Array Detector (HPLC-DAD) was developed for fingerprint analysis and quantitative determination of three major classes of constituent's namely phenolic acids, flavonoids and lignanoids. In the fingerprint analysis, nineteen peaks were selected as characteristic peaks and the chemical characteristics of three herbs in ZRG were presented in the HPLC chromatographic file. In the quantitative analysis, one flavonoid spinosin, four phenolic acids including danshensu, protocatechuic acid, protocatechuic aldehyde and salvianolic B and four lignanoids including schisandrin, gomisin A, deoxyschizandrin and gomisin N were successfully separated on an Ultimate™ XB-C 18 column (250 × 4.6 mm I.D., 5.0 μm) at 35°C. The mobile phase was acetonitrile-water (containing 0.03% phosphoric acid) employing a gradient elution at a flow rate of 1.0 mL/ min, and the detection wavelength was set at 280 nm. Regression equations revealed good linear relationship between the peak areas of the analytes and their concentrations (r > 0.9991) and the recoveries were in the range of 95.5~103.7%. The results indicated that the developed assay method could be considered as a suitable quality control method for ZRG. © 2010 Academic Journals.

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