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ABSTRACT: A novel, rapid and specific ultra performance liquid chromatography-photo diode array detection method was developed for the
simultaneous determination of 2,3,5,4′-tetrahydroxystilbene-2-O-β-d-glucoside (TSG), emodin-8-O-β-d-glucoside (EMG), emodin (EM) and physcion (PS). The chromatographic separation was performed on an Acquity BEH C18 column (100×2.1mm i.d., 1.7μm). The mobile phase was a mixture of 0.3% acetic acid–water and 0.3% acetic acid–acetonitrile
employing gradient elution at the flow rate of 0.4mLmin−1. The four compounds behaved linearly in the concentration range between 60.80–3040.00μgmL−1 (TSG), 0.50–25.00μgmL−1 (EMG), 2.16–108.00μgmL−1 (EM) and 1.56–78.00μgmL−1 (PS), respectively with correlation coefficients >0.999. The precision of the method were below 5% RSD. Recoveries of the
four compounds ranged from 95.71 to 102.97%, with RSD values less than 2%.
Chromatographia 04/2012; 70(3):657-659. · 1.20 Impact Factor
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ABSTRACT: Ultra high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC/ESI-Q-TOF-MS/MS) was applied to separate and identify triterpenoid saponins in crude extract from the stem bark of Albizia julibrissin Durazz. The molecular weights were determined by comparing quasi-molecular ions [M+NH(4)](+) in positive mode and [M-H](-) and [M-2H](2-) ions in negative mode. The MS/MS spectra of the [M-H](-) ions for saponins provided a wealth of structural information related to aglycone skeletons, sugar types and linked sequence. On the basis of the fragmentation behavior of known saponins isolated before, saponins from this plant were identified, even though references were not available. As a result, a total of twenty-eight saponins in the crude extract were identified, which all had a common basic skeleton of the triterpene oleanolic acid and eight of them were new compounds.
Journal of pharmaceutical and biomedical analysis 07/2011; 55(5):996-1009. · 2.45 Impact Factor
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ABSTRACT: Use HPLC to study the permeation of ingredients of Shuanghuanglian injection powder (SHL) through placental barriers of rats at different stages of pregnancy.
The pregnant rats were administered SHL for 5 d through caudalis vena at different stages of pregnancy. Plasma and embryonic tissues were obtained 12 h after the final administration of SHL. The componds in biological specimen were identified by HPLC.
Baicalin, luteolin and wogonoside were the main compounds in plasma. Wogonoside retained in first trimester embryonic tissues, and baicalin retained in the embryonic tissues of different pregnant stages.
Baicalin is the main compound of SHL through placental barriers of rats. Embryotoxicity of baicalin should be considered as the key point to evaluate the safety of SHL.
Zhongguo Zhong yao za zhi = Zhongguo zhongyao zazhi = China journal of Chinese materia medica 06/2010; 35(12):1626-9.
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ABSTRACT: A simple, sensitive and rapid LC-MS/MS method has been developed and validated for the identification and quantification of bivalirudin in human plasma using nafarelin as the internal standard. Following protein precipitation with methanol, the analytes were separated on a C(18) column interfaced with a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. Quantification of bivalirudin was conducted by multiple reaction monitoring (MRM) of the transitions of m/z 1091.4-->(356.4+227.4) for bivalirudin and m/z 662.4-->328.5 for IS. The lower limit of quantification was 1.25ng/ml, and the assay exhibited a linear range of 1.25-500ng/ml. The developed assay method was successfully applied to a pharmacokinetic (PK) study in healthy volunteers after intravenous administration of bivalirudin.
Journal of pharmaceutical and biomedical analysis 05/2010; 52(1):105-9. · 2.45 Impact Factor
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ABSTRACT: To identify the compounds in fruits of Psoralea corylifolia by high performance liquid chromatography-mass spectrometry.
The chromatographic separation was carried out at 30 degrees C on a Diamonsil C18 column (4.6 mm x 250 mm, 5 microm) eluted in the gradient program. The mobile phase consisted of acetonitrile (A) and water containing 0.05% formic acid (B). The detection wavelength was at 246 nm and the on-line UV spectra was recorded in the range of 190-400 nm. The mass spectra were obtained by Finnigan LCQ Deca XP(plus) ion trap mass spectrometer in the positive ion mode with ion spray voltage 4.5 kV, sheath gas (N2), 60 arbitrary units, auxiliary gas (N2), 20 arbitrary units; capillary temperature, 350 degrees C, capillary voltage 19 V, tube lens offset voltage 25 V, mass range recorded, m/z 90-800.
Two coumarin glycosides, three coumarins, eight flavonoids and one meroterpene were identified by HPLC-MS method.
The method is simple and rapid for the identification and quality control for the fruits of P. corylifolia.
Zhongguo Zhong yao za zhi = Zhongguo zhongyao zazhi = China journal of Chinese materia medica 11/2009; 34(22):2898-902.
