ABSTRACT
Objective: To compare the contents of three homoisoflavones and their anti-oxidative activity of Ophiopogon japonicus in Sichuan (OJS) and Zhejiang (OJZ). Methods: The determination was performed on ACQUITYTM UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm), the Ultra Performance Liquid Chromatography-Photo-Diode Array (UPLC-PDA) technology was applied, and the mobile phase consisted of acetonitrile and 0.2% formic acid aqueous solution (55:45) with gradient elution program, flow rate was 0.20 mL/min with 2 μL of sample quantity at 296 nm, and the anti-DPPH radical efficiency of water extract from Ophiopogonis Radix were evaluated by UV-photometer. Results: The average values of methylophiopogonone A, methylophiopogonanone A, and methylophiopogonanone B were (3.06±0.54), (40.10±5.63), and (29.51±5.06) μg/g in OJS, respectively; while those in OJZ were (9.22±3.52), (106.63±27.56), and (256.97±61.79) μg/g, separately. The IC50 value was 16.59 mg/mL in OJS, while that in OJZ was 14.48 mg/mL. The IC50 value of positive control VC was 7.06 μg/mL. Conclution: Compared with OJS, the contents of homoisoflavones in OJZ are higher, and the anti-radical efficiency of water extract from OJZ is stronger. It provides the basis for the quality evaluation and geo-authentic research of Ophiopogonis Radix.
ABSTRACT
Objective: To develop a UPLC-MS/MS method for simultaneously determining harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in Xuanmai Ganjie Granules (composed with Scrophulariae Radix, Ophiopogonis Radix, Glycyrrhizae Radix et Rhizoma, and Platycodonis Radix) from different pharmaceutical companies. Methods: The chromatographic separation was achieved on Phenomenex Kenetix C18 column (50 mm × 2.1 mm, 5 μm) by using a mobile phase consisted of acetonitrile and 0.1% formic acid water at the flow rate of 0.3 mL/min for gradient elution. Simultaneous monitoring of positive and negative ions and multiple reaction monitoring (MRM) scan mode were applied to the quantification of the components in Xuanmai Ganjie Granules; Sample volume was 5 μL. Results: There was good linearity between the absorption peak area and the concentration for harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in the ranges of 9-2250, 8-2000, 3.4-850, 96-24000, 12.4-3100, 3.6-1900, 1.7-425, and 1.5-375 ng/mL, respectively. The average recoveries were ranged from 97.2% to 102.8% (RSD ≤ 2.7%). The contents of harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in eight batches of samples were in the ranges of 32.8-107.6, 54.8-178.0, 14.6-70.7, 31.2-280.0, 106.4-287.9, 0.1-0.6, 0.01-0.07, and 0.03-0.17 μg/g, respectively. Conclusion: The developed method is simple, effective, and credible for determining the eight components in Xuanmai Ganjie Granules. It provides more helpful information for the comprehensive quality evaluation of Xuanmai Ganjie Granules.
ABSTRACT
Objective: To develop a liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneously analyzing seven components (ginsenosides Rg1, ginsenosides Re, ginsenosides Rb1, ophiopogonin D, ophiopogonin D', methylophiopogonanone A, and methylophiopogonanone B) in Shenmai Injection. Methods: Multiple reaction monitoring (MRM) scan mode was used for the quantification of five saponins and two flavones. The seven constituents were separated within 15 min on a Phenomenex Luna C18 column (150 mm × 2.1 mm, 5 μm) using a mobile phase consisted of acetonitrile and 0.03% acetic acid water solution with gradient elution. Results: The linear relationships between the concentration and peak areas of the seven target components were ginsenoside Rg1 Y=15.6 X + 1.63 × 104, ginsenoside Re Y=14 X + 5.36 × 103, ginsenoside Rb1 Y=2.46 X + 4.74 × 103, ophiopogonin D Y=11 X + 9.73 × 103, ophiopogonin D' Y=5.56 X + 1.64 × 103, methylophiopogonanone A Y=3.58 × 103 X + 2.33 × 104, and methylophiopogonanone B Y=4.87 × 103 X + 2.72 × 104, respectively. The precisions, repeatabilities, and stabilities of the method were good for the seven components. The average recovery ranged from 95.3%-104.3%, and the precision in terms of RSD was less than 2.4%. Conclusion: The method is rapid and reliable for the determination of the seven constituents in Shenmai Injection. Among these constituents, ophiopogonin D, ophiopogonin D', methylophiopogonanone A, and methylophiopogonanone B are quantified in the Shenmai Injection for the first time.
ABSTRACT
Objective To determine the contents of methylophiopogonanone A (MOA) and methylophiopogonanone B (MOB) in Radix Ophiopogonis and its extracts. Methods An HPLC-UV method was used for determining the contents of MOA and MOB in all samples. Analytical column was Kromasil C18 (250 mm?4.6 mm, 5 ?m). Mobile phase was acetonitrle-water (55∶45) and detection wavelength was 298 nm. The flow rate of mobile phase was 1 mL/min, and temperature was 30 ℃. Results The contents of MOA in Radix Ophiopogonis cropped in Sichuan and Zhejiang Provinces were 0.004 0%-0.009 6%, 0.006 7%-0.013 4%, and the contents of MOB were 0.002 1%-0.006 2%, 0.015 9%-0.028 2%, respectively. The contents of MOA in the extract of Radix Ophiopogonis cropped in Sichuan and Zhejiang Provinces were 0.007 5%-0.008 8%, 0.011 2%-0.012 6%, and the contents of MOB were 0.003 8%-0.005 1%, 0.020 7%-0.023 8%, respectively. Conclusion The contents of MOA and MOB in Radix Ophiopogonis cropped in Zhejiang Province and its extracts are more than those in Sichuan Province and its extrouts. The method can be used for the purpose of the quality control of Radix Ophiopogonis and its extracts.