ABSTRACT
This work describes the holistic fingerprinting method based on liquid chromatography coupled with charged aerosol detection(CAD) to profile non-saponin from water-soluble parts and determination of dencichine in Panax ginseng(PG), P. quinquefolium(PQ) and P. notoginseng(PNG). Sample extraction was carried out by water with ultra sonication for 30 min, which was eluted by Retain PEP for further analysis. The analysis was performed on a Hypercarb of porous graphitized carbon(3.0 mm×150 mm, 3 μm) column with acetonitrile and 0.1% perfluoropentanoic acid as mobile phase at a flow rate of 0.8 mL·min~(-1). Temperature of evaporator and nitrogen pressure for CAD were set at 50 ℃and 60.1 psi(1 psi≈6.895 kPa), respectively. As a result, dencichine and other polar components had a good performance on resolution and retention. The correlation coefficient(R~2) of dencichine was 0.998 2 in the concentration from 0.019 2 to 0.48 μg·mL~(-1). Limit of quantitation calculated by signal to noise of 10 was 7.4 ng·mL~(-1), and the recovery ranged from 95.52% to 102.7%. Chemical profile of the water-soluble part from PG, PQ and PNG was similar holistically, while the relative content for dencichine and other partial components varied significantly. The proposed method was used for characteristic of chemical profiling for non-saponin from water-soluble part, and determination of dencichine in PG, PQ and PNG.
Subject(s)
Aerosols , Amino Acids, Diamino , Chromatography, High Pressure Liquid , Chromatography, Liquid , Panax , Panax notoginseng , Plant Roots , Saponins , WaterABSTRACT
Ginsenoside Ro decreased measures of inflammation, aging, oxidants and thrombus formation in a previous study. To measure ginsenoside Ro content in red ginseng from different years, an optimized extraction method was developed to determine ginsenoside Rg1, Re, Rb1 and Ro content by HPLC in 43 batches of red ginseng from different origins, growing years and manufacturers. The results indicate that the best extraction method was to ultrasonify a 1 g sample in 70% methanol for 50 min. The total running time of the optimized gradient was 50 min using a C18 core-shell column and was half the time described in the Chinese Pharmacopoeia, 2015 edition. The separation resolution of all of targeted compounds was greater than 1.6. The peak shape of ginsenoside Ro was optimal when the mobile phase consisted of acetonitrile and water with 0.1% phosphoric acid. The content of ginsenoside Ro was in the range of 0.11% to 0.43%, and the average content was 0.26%, which was higher than that of ginsenoside Rg1 and Re. The ratio of ginsenoside Ro and Re as a threshold could be used to discriminate red ginseng from different growing years; in addition, 100%, 94.4% and 46.6% of red ginseng from six, five and four years exceeded the threshold of 1.3. Our optimized analytical method for characterization of red ginseng is convenient and shortens the assay time.
ABSTRACT
We have developed a new method using HPLC-CAD (charged aerosol detector) for the quantitative analysis of cyclovirobuxine D and related substances in the API of Huangyangning tablets. The related substances were further studied by HPLC-Q-Exactive coupled with hybrid quadrupole-orbitrap mass spectrometry. A HILIC column of XBridge Amide (4.6 mm×250 mm, 5 μm) was used, and the mobile phase was composed of acetonitrile and 100 mmol·L-1 ammonium formate (85∶15), which was adjusted to pH 2.8 with formic acid. Isocratic mode elution was adopted at a flow rate of 1.1 mL·min-1. The column temperature was set at 30 ℃. For CAD, the temperature of atomization and gas pressure were respectively set at 35 ℃ and 62.2 psi. This method detected and quantified five related substances to cyclovirobuxine D. The results showed that the LOD and LOQ of cyclovirobuxine D was 12.588 ng and 28.323 ng, respectively with an average recovery of 95.74% (RSD = 1.79%, n = 6). The content of cyclovirobuxine D in 12 batches of API samples provided by three manufacturers was from 79.94% to 88.49%, with an average value of 82.20%. The total content of the five related substances was from 15.99% to 22.15% with an average value of 20.10%, using an external standard method with cyclovirobuxine D as the reference and according to the CAD uniform response to non-volatile substances. The newly developed HPLC-CAD method has advantages in terms of the comprehensiveness of signals from Buxus alkaloids without UV absorption and with high sensitivity to its trace-related substances; the method yields good separation between the components and is compatible with mass spectrometry. It is applicable for the accurate quantitative analysis of main components and related substances in the API of Huangyangning tablets.
ABSTRACT
Objective: To establish a rapid method for the simultaneous quantification of eight ginsenosides in Notoginseng Radix et Rhizoma (NRR), Ginseng Radix et Rhizoma (GRR), and their related products by multi hearting-cutting two dimensional liquid chromatography based a "monomethod-heterotrait matrix" (MHM) strategy. Methods: Corresponding sample preparations were applied to samples, which were different in either product forms or preparation processes. Pressured liquid extraction (PLE) was developed for the raw herbs and related solid-state Chinese patent medicine using two-steps solvent extraction with chloroform and water-saturated n-butanol. One and two dimensional separation conditions including columns selection and gradient elution were optimized systematically. Phenyl-X and C18 were confirmed as 1D and 2D columns, respectively. Eight targeting ingredients were cut alternately into six loops by starting-to-ending time of peaks in 1D column. 2D rapid separation for eight cycles was achieved on core-shell column with 2.6 μm particle to complete eight compounds quantitation. Results: The eight targeting analytes were well separated and quantified in 50 min in different sample matrix (raw herbs, extract, and Chinese patent medicine). Method validation was performed in terms of linearity (r ≥ 0.999), precision (0.52%-1.53%), and recovery (ranged from 94.57% to 103.47%), and the LODs (S/N=3:1) of the eight analytes varied from 0.041 to 0.18 μg/mL respectively. Conclusion: Eight ginsenosides could be quantified accurately for different sample matrix. Combined with its relative proportions of eight ginsenosides, quality evaluation for NRR, GRR, and their related products could be performed scientifically.
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There is a certain correlation between glioma and depression,both of which belong to brain diseases. Glioma pa?tients often have comorbid depression which is not conducive to the treatment of glioma. By retrieving a large number of domestic and foreign literature,we found antidepressants can efficiently prevent and treat glioma,but the treatment mechanism is not clear. Through analyzing the correlation between depression and glioma on clinical features,pathological characteristics and traditional Chi?nese medicine theory,this paper reviews the research progress on the mechanism of anti-depression drugs against glioma. It aims to provide a reference for anti-glioma drugs screening and new ideas for exploration of treatment strategy of glioma.
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To establish the online two-dimensional liquid chromatography by using double gradient liquid chromatography system and UV detector, in order to simultaneously determine the content of paeoniflorin, paenol, amygdaloside and cinnamic acid. A pump of the two-dimensional liquid chromatography was adopted as the one-dimensional separation pump. C18 (3.0 mm x 150 mm, 3 microm) was used as the analytical column, with acetonitrile as the organic phase and 0.08% phosphoric acid + 0.08% triethylamine as the aqueous phase for gradient elution at the flow rate of 0.5 mL x min(-1). Another pump of the two-dimensional liquid chromatography was adopted as the two-dimensional separation pump. PAII C18 was used as the analytical column, with acetonitrile as the organic phase and 20 mmol, pH 3.0 monopotassium phosphate as the aqueous phase for gradient elution at the flow rate of 0.8 mL x min(-1). The detection wavelengths were set at 218, 230, 275 nm by using wavelength time-switching program. The linearity range of paeoniflorin, amygdaloside, paeonol and cinnamic acid were 5.55-222 (r = 0.999 7), 6.6-264 (r = 0.999 8), 3.3-132 (r = 0.999 5) and 0.315-12.6 mg x L(-1) (r = 0.999 7), respectively. The average recoveries of the four components were between 96.12% and 103.9%. The experiment proved that this method was so rapid and accurate in determination results that it could be used for evaluating drug quality.