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Liang X.,Shenyang Pharmaceutical University | Tian J.,Shenyang Pharmaceutical University | Li L.,Shenyang Pharmaceutical University | Gao J.,Liaoning Chengda Biotechnology Co. | And 3 more authors.
Talanta | Year: 2014

A rapid and reliable microwave extraction and the triple quadrupole-linear ion trap mass spectrometry method was developed and validated for the determination of eight alkaloids in Portulaca oleracea L. The optimal microwave extraction (MWE) condition was performed at 60 °C for 12 min with ethanol-water (70:30, v/v) as the extracting solvent, and the solvent to solid ratio was 30:1. The alkaloids were first detected simultaneously by electrospray ionization tandem mass spectrometry under positive-negative conversion multiple reaction monitor ((+/-)MRM) technique. With investigating three different columns, samples were separated in only 8 min on a Waters ACQUITY UPLC HSS T3 (50×2.1 mm2, 1.8 μm) column using acetonitrile and formic acid-water solution as a mobile phase with a flow rate at 0.2 mL/min. All calibration curves showed good linearity (r>0.999) within the test ranges. The method developed was validated with acceptable sensitivity, intra- and inter-day precision, reproducibility, and extraction recoveries. It was successfully applied to the determination of eight alkaloids in Portulaca oleracea L. from different sources and different harvest periods. The method also provide a reference for extraction and determination of alkaloids in other complex systems. © 2013 Elsevier B.V. All rights reserved.


Liang X.,Shenyang Pharmaceutical University | Li L.,Shenyang Pharmaceutical University | Tian J.,Shenyang Pharmaceutical University | Wu Y.,Shenyang Pharmaceutical University | And 4 more authors.
Phytochemical Analysis | Year: 2014

Introduction - Portulaca oleracea L. (P. oleracea, purslane) is an edible plant that is widely distributed around the world, and flavonoids are its main bioactive constituents. Therefore, the detection of flavonoids is very important for a better understanding of its pharmacological actions and to monitor the product quality control of P. oleracea.Objective - To develop a rapid method to extract and determine 26 bioflavonoids in P. oleracea, based on microwave extraction (MWE) and triple quadrupole-linear ion trap mass spectrometry.Methods - The optimal conditions of MWE for the extraction of flavonoids from P. oleracea involved the use of methanol as the extraction solvent, a microwave power of 300 W, an extraction time of 450 s, and a solvent-to-solid ratio of 30 mL/g. The samples were analysed using an ultra-performance liquid chromatograph coupled with a triple quadrupole-linear ion trap mass spectrometer (UPLC-MS/MS) system.Results - The calibration curves of all 26 analytes showed good linearity (r = 0.999) and the intra- and interday precisions and repeatability were all within required limits. The mean recoveries measured at three concentrations were higher than 94.2%, with RSDs lower than 2.94% for the targets.Conclusion - The established MWE/UPLC-MS/MS method is a rapid and effective method for quality evaluation of P. oleracea from different production regions and different harvest periods. © 2014 John Wiley & Sons, Ltd.


Yang J.,Liaoning Chengda Biotechnology Co. | Gao J.,Liaoning Chengda Biotechnology Co. | Zhang Q.-Y.,Liaoning Chengda Biotechnology Co.
Chinese Journal of Biologicals | Year: 2010

Objective To develop a gas chromatography for determination of β-propiolactone (BPL) content and analyze the hydrolysis of BPL. Methods Gas chromatography was used for determination of BPL content, then evaluated for linear range and detection limit, and verified for reproducibility and specificity. The tendency of BPL hydrolysis at 37t was analyzed. Results The developed gas chromatography for BPL showed a linear range of 8. 9 ∼ 566. 9 ppm, a detection limit of 8. 9 ppm, and high reproducibility and specificity. After hydrolysis at 37°C for 120 min, the BPL content decreased to the 19% of original one. Conclusion A gas chromatography for determination of BPL content was developed, which was accurate, reliable and might be used for determination of BPL content during production of viral vaccines. It provided a basis for verification of virus inactivation procedure.

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