Determination of 14 components in Bazibushen capsule by UPLC-ESI-MS/MS / 药学学报

The study developed a method for the determination of 14 components in Bazibushen capsule by UPLC-ESI-MS/MS. Waters ACQUITY BEH C18 column (50 mm×2.1 mm, 1.7 μm) was used and the column temperature was 40℃. A linear gradient elution of eluents A (acetonitrile) and B (0.1% acetic acid) was used for the separation. The source temperature was set at 150℃. The capillary voltage was set at 2.0 kV. The source offset voltage was kept at 50 V. The desolvation temperature was set at 500℃. The desolvation flow was 800 L·h-1. The cone flow was 150 L·h-1. The nebuliser pressure was 7.0 Bar. Multiple reaction monitoring mode (MRM) is adopted. All of the 14 components showed good linearity (r2 > 0.999 1) in the test ranges. The LOQs for the compounds ranged from 0.11-4.52 ng·mL-1, respectively. The RSDs were 0.8%-2.1%. The overall recoveries were between 97.89% and 101.9% for all compounds. The method is simple, rapid, accurate and highly reproducible, and may be used in the determination of 14 components in Bazibushen capsule.

Simultaneous quantification of 7 coumarins in common cnidium fruit by GC-MS / 药学学报

A GC-MS-SIM method was developed for the simultaneous determination of the 7 coumarins in common cnidium fruit. The 7 bioactive constituents were separated on DB-1 capillary column (30 m×0.25 mm, 0.25 μm) using temperature programming. The interface temperature was set at 280℃; Ion source temperature:250℃; Quadrupole temperature:150℃; EI mode:70 eV; The mass spectrometer detector was in SIM mode; Scan range:50-350 amu. All the 7 marker substances showed good linearity (r2>0.9986) in the test ranges. The LODs and LOQs for the compounds ranged from 1.06 to 10.11 ng ·mL-1 and from 3.21 to 29.88 ng·mL-1, respectively. The overall intra-day (n=6) and inter-day (n=3) RSDs were 0.7%-2.5% and 1.2%-3.3%, respectively. The overall recoveries were between 92.38% and 100.50% for all compounds. This method was simple, rapid, sensitive, with good specificity, and it can provide a reference for the quality control of common cnidium fruit.

Simultaneous determination of 4 diterpenoids in Rabdosia japonica var.glaucocalyx by HPLC-ESI-MS/MS and cluster analysis / 中国中药杂志

A quick HPLC-ESI-MS/MS method was established for simultaneous determination of four major diterpenoids in Rabdosia japonica var.glaucocalyx, including glaucocalyxin A, oridonin, hebeirubesensin and enmenol. Analysis was performed on an Agilent ZORBAX SB-C18(4.6 mm×250 mm, 5 μm ) column eluted in a gradient program with methanol and water. The flow rate was 0.8 mL•min⁻¹. Multiple reaction monitoring (MRM) scanning mode was performed in negative ion switching mode to apply for the quantitative determination. The calibration curves for the above four compounds were linear in corresponding injection amount. The average recoveries of the compounds ranged from 92.40% to 105.9%, with RSDs of 1.7%-6.5%. The method is simple, rapid, accurate with good repeatability, which can provide a reference for overcalling evaluation the quality of R. japonica var.glaucocalyx. The result of cluster analysis- showed that the quality of R. japonica glaucocalyx var. greatly varied between areas and parts.

Simultaneous determination of 3 phenolic acids in Usnea by HPLC-ESI-MS/MS / 中国中药杂志

A quick HPLC-ESI-MS/MS method was established for simultaneous determination of three chemical compositions in Usnea, including usnic acid, diffractaic acid, and ramalic acid. The separation was performed on a chromatographic column of Agilent ZORBAX SB-C, (4.6 mm x 250 mm, 5 µm), and the mobile phase was methanol (0.05% formic acid)-0.05% formic acid solution (4 mmol ammonium acetate), with an isocratic elution at a flow rate of 0.8 ml · min⁻¹. Multiple reaction monitoring scanning mode (MRM) was performed combined with the ion switching technology in positive and negative ion switching mode to apply for the quantitative determination. The calibration curves for the above three compounds were linear in corresponding injection amount. Their average recoveries were 95.0%-105.1%, with RSDs of 1.1%-5.2%. The method was simple, rapid, accurate with high repeatability, which could provide a reference for overcalling evaluation the quality of Usnea.

Study on the metabolite of stilbene glucoside in mice by liquid chromatography tandem-mass spectrometry / 药学学报

<p><b>AIM</b>To study the metabolite of stilbene glucoside in the Chinese traditional medicine Polygonum multiflornm in mice and elucidate its chemical structure by liquid chromatography tandem-mass spectrometry.</p><p><b>METHODS</b>The stilbene glucoside was injected into the tail vein of mice. Blood samples were collected from artery in the eyepit. The methanol-protein-precipitated plasma sample was introduced into the liquid chromatography-tandem mass spectrometer directly. The analytical column was C18 column (250 mm x 4.6 mm ID, 5 microns). The mobile phase consisted of acetonitrile-methanol-water-formic acid (15:18:66:1) for ES+, acetonitrile-methanol-water (15:18:67) for ES-. The UV detection wavelength was set at 320 nm. The mass ion source type was ESI. HV capillary was 3 kV. The dry gas was nitrogen gas and the flow rate was set at 318 L.h-1. The ion source temperature was 150 degrees C.</p><p><b>RESULTS</b>The stilbene glucoside and its metabolite were separated completely under the chromatography condition. The ions at m/z 600 and m/z 605 were detected under positive ion polarity while the ions at m/z 581 and m/z 402 were detected under negative ion polarity.</p><p><b>CONCLUSION</b>It was proposed that the metabolite of stilbene glucoside injected in vein was its glucuronide conjugate.</p>

Studies on pharmacokinetics of loganin and morroniside in Cornus officinalis injection in mice / 中国中药杂志

<p><b>OBJECTIVE</b>To establish a revered-phase HPLC method for the study of pharmacokinetics of loganin and morroniside in Cornus officinalis injectionin mice after a single oral and intravenous administrations.</p><p><b>METHOD</b>The Diamonsil C18 column (4.6 mm x 250 mm, 5 microns) was used as the analytical column and the mobile phase consisted of acetonitrile-methanol-0.2% formic acid (12:8:80) with the flow rate at 1.0 mL.min-1. The UV detection was set at 237 nm.</p><p><b>RESULT</b>The calibration curves of loganin and morroniside were linear in the range from 0.38 to 68.25 mg.L-1(r = 0.9999), and from 0.66 to 117.22 mg.L-1(r = 0.9999), respectively. The lowest determination concentrations of loganin and morroniside were 0.10 and 0.16 mg.L-1, respectively. The recoveries and relative standard deviations of loganin were 99.6% (2.0%), 102.0% (1.0%), 87.9% (7.2%), and those of morroniside were 99.2% (2.5%), 104.1% (1.2%), 92.7% (4.2%), respectively. The relative standard deviations of within-day and between-day precision for the method were all less than 6.8%. After a single intravenous administration of Cornus officinalis injection to mice, the mean plasma concentration-time courses were found to fit a two-compartment open model, the main pharmacokinetic parameters of loganin were as follows: T1/2(alpha), T1/2(beta), K21, K12, K10, V(c), AUC, CL were 3.2 min, 25.1 min, 5.997 h-1, 4.981 h-1, 3.564 h-1, 0.551 L.kg-1, 13.59 mg.L-1.h, 1.965 L.kg-1.h-1, respectively and those of morroniside were 3.6 min, 21.5 min, 5.926 h-1, 3.833 h-1, 3.797 h-1, 0.647 L.kg-1, 27.15 mg.L-1.h, 2.457 L.kg-1.h-1, respectively.</p><p><b>CONCLUSION</b>It is the first time to establish the revered-phase HPLC method to determine concentrations of loganin and morroniside in plasma and to obtain their pharmacokinetic parameters and characteristics.</p>

Fingerprints of genuine Radix Polygalae from Hebei Province with HPLC-UV / 中草药

Objective To establish HPLC-UV fingerprints of genuine Radix Polygalae from Hebei Province and get the control fingerprint.To compare the fingerprints of genuine Radix Polygalae collected from different habitats with the control fingerprint so as to establish a specific method for the quality con- trol of genuine Radix Polygalae.Methods The fingerprints of 19 batches of genuine Radix Polygalae were obtained from Waters 1525 pump.The chromatographic procedure was carried out with Diamonsil~(TM) C_(18)(250 mm)?4.6 mm,5?m)as an analytic column and a mixture consisting of acetonitrile and 0.2% formic acid in gradient as mobile phase.The detection wavelength was 316 nm.The flow rate was 1.0 mL/min.The temperature of column was 35 C.Results The control fingerprint of HPLC-UV was set up.The fingerprints of genuine Radix Polygalae from different habitats were compared.Conclusion The operation of this method is simple,quick,accurate,and could be used for the identification and quality control of genuine Radix Polygalae.