Terpenoids from leaves of Chinese hawthorn / 中国中药杂志

Fifteen compounds were isolated from the 70% EtOH extract of leaves of Chinese hawthorn(Crataegus pinnatifida var. major) by various purification steps, and their structures were determined as 2α,3α,12β,19α,-tetrahydroxyursan-13β,28-olide(1),euscaphic acid(2), tormentic acid(3), ursolic acid(4), pomolic acid(5), corosolic acid(6), maslinic acid(7), linalyl rutinoside(8),(Z)-3-hexenyl β-D-glucoside(9),(3S, 6S)-cis-linalool-3,7-oxide-β-D-glucopyranoside(10), pisumionoside(11), icariside B6(12), byzantionoside B(13),(6R,7E,9R)-9-Hydroxy-4,7-megastigmadien-3-one 9-O-β-D-glucopyranoside(14) and(6S,7E,9R)-6,9-dihydroxy-4,7-megastigmadien-3-one 9-O-β-D-glucopyranoside(15) mainly based on the mass spectrum(MS) and nuclear magnetic resonance(NMR) spectroscopic techniques, of which compound 1 was a new pentacyclic triterpene, and compounds 2, 5, 6, 8, 10, 13 and 15 were isolated form this plant for the first time.

Experimental study on inhibitory effect of hawthorn leaves flavonoids on human glioblastoma U87 cells / 中国药理学通报

Aim To explore the inhibitory effect of hawthorn leaves flavonoids (HLF) on human glioblastoma U87 cells. Methods U87 cells were cultured in vitro. The concentration of HLF was 25, 50, 100 mg . L¹ as drug concentration. The effects of HLF on the proliferation, migration, invasion and adhesion of U87 cells were detected by CCK-8 assay, scratch assay, Transwell assay and adhesion assay, and clone forming ability was detected by cell clonogenic assay. Results HLF inhibited the proliferation, migration, invasion and adhesion of U87 cells in a concentration-dependent manner, and the difference was statistically significant compared with control group (P < 0. 05). When HLF reached 50 mg . L¹ the inhibition of tumor growth was the most significant. Conclusion HLF has a certain inhibitory effect on glioma U87 cells.

Research on equilibrium solubility and apparent oil/water partition coefficient of flavonoids components in hawthorn leaves by similarity analysis / 中草药

Objective To study the equilibrium solubility and oil/water partition coefficient of Hawthorn leaves flavonoids (HLF) components, and compare their similarity, to lay the foundation for the characterization of the overall water soluble and fat soluble HLF components. Methods Taking HLF components as model drug, rutin, quercetin, and hyperin as representative components. The HPLC method was used to determine the equilibrium solubility and apparent oil/water distribution coefficient (Papp) of the components at different pH values and water. The similarity was evaluated by the vector cosine method (cosines) and Grubbs method (Grubbs). Chromatographic conditions: The chromatographic column was Zorbax Eclipse Plus C18 column (250 mm × 4.6 mm, 5 μm), and the flow phase was acetonitrile (A) - 0.4% phosphate solution (B). The gradient elution program was 0—10 min (80% B), 10—11 min (80%—60% B), 11—20 min (60% B), 20—21 min (60%—80% B), and 21—25 min (80% B); The detection wavelength was 360 nm; The volume flow was 0.8 mL/min; The column temperature was 40 ℃. Results The equilibrium solubility and Papp of rutin, quercetin, hyperin were similar in different pH buffer solution and water. The solubility value of lutin, quercetin, and hyperoside in thebuffer solution of different pH were 0.998, 0.988, and 0.987, respectively. The cosine value of the apparent oil-water distribution coefficient was 0.976, 0.981, and 0.978, respectively. The cosine value was greater than 0.9. The Grubbs value of equilibrium solubility of lutin, quercetin and hyperoside were 1.057, 1.083, 1.124, 1.117, 1.022, 1.030, 1.082, and 1.112, respectively. The Grubbs values of the apparent oil-water distribution coefficient were 1.125, 1.107, 1.079, 1.034, 1.041, 1.037, 1.129, and 1.128. The results of Grubbs were less than G critical value of 1.153, and the similarity was good. Conclusion The similarity analysis reflects that the degree of dispersion of components objectively, which could increase the science of components evaluation and provide the basis for the formulation design of components of traditional Chinese medicine.

Key physical parameters of hawthorn leaf granules by stepwise regression analysis method / 中国中药杂志

The purpose of this study was to investigate the effect of key physical properties of hawthorn leaf granule on its dissolution behavior. Hawthorn leaves extract was utilized as a model drug. The extract was mixed with microcrystalline cellulose or starch with the same ratio by using different methods. Appropriate amount of lubricant and disintegrating agent was added into part of the mixed powder, and then the granules were prepared by using extrusion granulation and high shear granulation. The granules dissolution behavior was evaluated by using equilibrium dissolution quantity and dissolution rate constant of the hypericin as the indicators. Then the effect of physical properties on dissolution behavior was analyzed through the stepwise regression analysis method. The equilibrium dissolution quantity of hypericin and adsorption heat constant in hawthorn leaves were positively correlated with the monolayer adsorption capacity and negatively correlated with the moisture absorption rate constant. The dissolution rate constants were decreased with the increase of Hausner rate, monolayer adsorption capacity and adsorption heat constant, and were increased with the increase of Carr index and specific surface area. Adsorption heat constant, monolayer adsorption capacity, moisture absorption rate constant, Carr index and specific surface area were the key physical properties of hawthorn leaf granule to affect its dissolution behavior.

Simultaneous Determination of Four Flavonoids in Extract of Hawthorn Leaves by Microemulsion Liquid Chromatography / 分析化学

A novel system was developed for the rapid determination of vitexin, vitexin-2″-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn(Crataegus pinnatifida Bge.) leaves with microemulsion liquid chromatography(MELC). The effect on the chromatography of varying the operating paramers was studied. The optimized MELC system with microemulsion was consisting of 1.0%(w/w) brij35-1.1%(w/w) n-butanol-0.1%(w/w) n-octanol-0.3%(v/v) triethylamine, the pH was adjusted to 2.5 with phosphoric acid. The type and concentration of surfactant, types of oil phase, the pH and triethylamine as the organic additive in microemulsion played an important role for separation of four flavonoids. MELC analysis was performed on a Venusil ASB C_(18) analytical column (150 mm× 4.6 mm, i.d., 5 μm). The flow rate was set at 0.8 mL/min and the eluent was detected at 340 nm for the four flavonoids. The calibration curves of the four flavonoids are linear(r>0.9995) over the concentration range of 0.95-140.0 mg/L. The mean recoveries are 98.6% to 101.6%. The results indicate that the optimized method was successfully applied to the analysis of four important flavonoids in the extract of hawthorn leaves.

Comparative analysis of ursolic acid in Hawthorn leaves by HPLC / 中成药

AIM: To develop a simple HPLC for the determination of ursolic acid in Hawthorn leaves, and to compare ursolic acid content in Hawthorn leaves of different species, locations and growth stages, so as to supply some evidences for the exploitation and utilization of Hawthorn leaves reasonably. METHODS: By high-performance liquid chromatography method. Lichrospher C18 column (250 ×4.6 mm I. D. 5 μm); mobile phase, acetonitrile-water-orthophosphoric acid (85: 14.95: 0.05) with a flow-rate of 1.00 ml/min; column temperature at 30 ℃; injection volume, 5μl; UV detector at 210 nm. RESULTS: The detection limit (S/N=3) was less than 4. 024 μg/ml and the limit of quantification( S/N =10) was less than 12.05 μg/ml. The calibration curve showed good linear regression(r =0. 9999) within measurement ranges( 16.09 - 1030 μg/ml). The intra-day and interday variation were 0.71% and 6. 15%, respectively. The recoveries at low to high concentration were 89%-105%. Under these conditions, the ursolic acid content in different Hawthorn leaves were determined: 1.90%-1.95% in C. scabrifolia (Franch.) Rehd, 1.00%-1.45% in C. cuneata Sieb. & Zucc, 0.45%-0.65% in C.pinnatifida Bge. var. major N. E. Br.; In differnet growth stages of C. pinnatifida Bge. var. major N. E. Br. , the young leaves contain higher content of ursolic acid. CONCLUSION: The method is successfully applied to quantify ursolic acid in Hawthorn leaves. And the ursolic acid contents in Hawthorn leaves of differnent species are very different; C. scabrifolia (Franch.) Rehd contains the highest ursolic acid content in them. However, there is a little difference among different locations and growth stages for same species.

Self-microemulsifying drug delivery system of flavonoids in hawthorn leaves / 中草药

Objective To develop the formulation of self-microemulsifying drug delivery system for hawthorn leaves flavonoids (HAW-SMEDDS). Methods The optimum formulations of oil phase, surfactant, and assistant surfactant for HAW-SMEDDS were screened by solubility test, compatibility test, and pseudo-ternary phase diagrams, with the time of formulating microemulsion, the consequence of visual examination, and particle size as indexes. The dissolution of HAW-SMEDDS was measured, taking the commercial tablet Yixintong Tablet as reference. Results The optimum self-microemulsifying drug delivery system was composed of Labrasol (35%), Transcutol P (10%). The particle diameter was (39.5?5.4) nm, the time of self-microemulsifying was less than 1 min. The percent of accumulated dissolution of hawthorn leaves flavonoids in SMEDDS in distilled water was up to 70% at 10 min, while that in the Yixintong Tablet was less than 50% at 60 min. Conclusion The formulation of HAW-SMEDDS preparation could meet the request of the design. It could provide the reference for the new dosage form.

In situ rat intestinal absorption of hawthorn leaves flavonoids / 中成药

0.05).But the P_ eff values were significantly increased in the presence of P-glycoportein(P-gp)inhibitor,verapamil or digoxin.CONCLUSION:Rhamnosylvitexin can be classified into high penetrating drug.Passive diffusion dominates the absorptive transport behavior of rhamnosylvitexin in HLF.There is not a preferential absorption zone in the intestine for rhamnosylvitexin.The absorption and secretion of rhamnosylvitexin in HLF are mediated by the efflux transport system,P-gp.

HPLC fingerprint chromatogram of leaves of Hawthorn / 中成药

AIM: To establish HPLC fingerprint chromatogram of leaves of Hawthorn and to evaluate the constituents and to provide the basis for identification. METHODS: Leaves of Hawthorn come from 10 production places were analysed to gain its contents,such as Vitexin,Hyperoside,2″-O-Rhamnosylvitexin,Rutin,4-O-Rhamnosylrutin,Chlorogenic acid,Quercetin 3-O-?-glucoside,4-O-Glucosylvitexiu,and internal reference selected Chlorogenic acid. RESULTS: The different leaves of Hawthorn showed different HPLC chromatogram. CONCLUSION: HPLC chromatogram can be used to distinguish the leaves of different species of Hawthorn and the content of the main characteristic components are various as production places vary.