OBJECTIVETo develop an LC-MS method for identification of flavonoids in Chinese hawthorn fruits and an HPLC method for quantification of 5 flavonoids.

METHODAccurate molecular weights of the target flavonoids were acquired by time-of-flight mass spectrometer (TOF-MS) in both positive and negative ion modes. The flavoniods were then further confirmed by standards. An RP-HPLC method was established to quantitatively analysis five major flavonoids (chlorogenic acid, procyanidin B2, epicatechin, hyperoside and isoquercitrin) in hawthorn fruits from ten different regions.

RESULTSThe molecular formulae of 8 components were determined by TOF-MS. In the quantitative method validation, the method is linear over the studied range of 1.8-178.5, 2.2-284.8, 2.7-270. 6,1.5-150.0, 1.5-150.0 mg x L(-1) for chlorogenic acid, procyanidin B2, epicatechin, hyperoside and isoquercitrin, respectively. The correlation coefficient for each analyze was greater than 0.999. The inter-day precision of the analysis was lower than 4%, The RSDs of precision and stability were lower than 5%. The recovery rate was from 98.5% to 102.5%, and RSDs were less than 3.5%.

CONCLUSIONThe method is simple, specific and reliable, and is suitable for quality control of Chinese hawthorn.

Chromatography, High Pressure Liquid ; methods ; Crataegus ; chemistry ; Flavonoids ; analysis ; Fruit ; chemistry ; Mass Spectrometry ; Quality Control

OBJECTIVETo study the hypolipidemic active compounds from Crataegus pinnatifida and mechanism of action of those.

METHODGuided by the inhibitory activity to HMG-CoA reductase, the active compounds were separated and purified with macroporous resin and silica gel.

RESULTFour active compounds were obtained, which were quercetin, hyperoside, rutin and chlorogenic acid, the sum of their inhibitory rate was 50.01%, and the total inhibitory rate of the mixture of four active compounds matched was 79.48%.

CONCLUSIONQuercetin and hyperoside were the principle active components inhibiting HMG-CoA reductase in Hawthorn fruit, and there were synergistic action among them.

Crataegus ; chemistry ; Fruit ; chemistry ; Hydroxymethylglutaryl CoA Reductases ; analysis ; Hydroxymethylglutaryl-CoA Reductase Inhibitors ; pharmacology ; Plant Extracts ; pharmacology

OBJECTIVETo study the technical conditions of the extraction and purification of the active composition from Polygonum orientale and Crataegus pinnatifida Bge. in Hongye Xingtong soft capsules with the macroporous resin.

METHODThe orientm, isorientm and hyperoside were used as index to screen the five kinds of resins. And the technical conditions of the enrichment and purification of D101 resin selected out of above were all-round studied.

RESULTThe D101 was fit for adsorbing orientm, isorientm and hyperoside. Under the optimal conditions, the transfer rate of orientm, isorientm and hyperoside was above 91%, and the total solid was cut down by more than 60%.

CONCLUSIONThe D101 is greatly effective for the enrichment and purification of the active composition of P. orientale and C. pinnatifida Bge.

Crataegus ; chemistry ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Polygonum ; chemistry ; Quercetin ; analogs & derivatives ; chemistry ; isolation & purification ; Resins, Synthetic ; chemistry

OBJECTIVETo evaluate the stability of physical state with accelerate test and dropping in process before and after on compound hawthorn dropping pills.

METHODScanning electron microscope, TG-DTA, FT-IR and XRD were used.

RESULTThe active components presented amorphous, tiny crystal and molecular state in dropping pills, and it had no obvious reaction between PEG 4000 and active components. With time prolonging, a little of active components changed from amorphous state to tiny crystal or molecular state.

CONCLUSIONSolid dispersion improved the stability and dissolution of compound hawthorn dropping pills.

Crataegus ; chemistry ; Drug Compounding ; methods ; Drug Stability ; Drugs, Chinese Herbal ; chemistry ; Microscopy, Electron, Scanning ; Solubility ; Spectroscopy, Fourier Transform Infrared

To prepare the hawthorn leaves flavonoids self-microemulsifying membrane controlled-release coated drop pill, and to study its release rate in vitro and pharmacokinetics study in vivo. In order to improve the dissolution of hawthorn leaves flavonoids, self-microemulsifying technology was used to prepare the hawthorn leaves flavonoids self-microemulsion. Hawthorn leaves flavonoids self-microemulsifying drop pill was prepared with the PEG 6000. Studies were made on the in vitro release of flavonoids from hawthorn leaves self-micro-emulsifying membrane-moderated coated drop pills and the in vivo pharmacokinetic in rats. The prescription of flavonoids from hawthorn leaves self-micro-emulsifying drop pills was 0.25 g of flavonoids from hawthorn leaves, 0.25 g of iodophenyl maleimide, 0.375 g of polyethylene glycol 400, 0.375 g of cremophor RH 40 and 2 g of polyethylene glycol 6000. The optimized prescription was 4 g of ethyl cellulose 20, 0.64 g of polyethylene glycol 400, 1.8 g of diethyl phthalate, and the weight of coating materials increased by 3.5%. Flavonoids from hawthorn leaves self-micro-emulsifying membrane-moderated coated drop pills complied with the design of sustained-release in 12 h in terms of in vitro release and in vivo pharmacokinetic parameters in rats, and its bioavailability was 2.47 times of quick-release drop pills. Slightly soluble flavonoids from hawthorn leaves could be made into sustained-release preparations by the self-micro-emulsifying and coating technology.
Animals ; Chemistry, Pharmaceutical ; Crataegus ; chemistry ; Delayed-Action Preparations ; chemistry ; pharmacokinetics ; Drugs, Chinese Herbal ; chemistry ; pharmacokinetics ; Flavonoids ; chemistry ; pharmacokinetics ; Male ; Plant Leaves ; chemistry ; Rats ; Rats, Sprague-Dawley

OBJECTIVETo develop an HPLC method for determining flavoniod-glycosides in Yixintong pills.

METHODAgilent ZORBAX Extend-C18 (4.6 mm x 250 mm, 5 microm) was used with tetrahydrofuran-methanol-acetonitrile-water-acetic acid (30:3:4:120:3) as mobile phase. Detection wavelength was 330 nm.

RESULTGood linearities of rhamnosylvitexin and vetexin-glucoside were obtained within the range of 0.044-1.78 microg (r = 0.9999) and 0.042-0.85 microg (r = 0.9999); the average recoveries were 100.0% and 99.2%; RSD were 0.92% and 1.8%, respectively.

CONCLUSIONThis method can be used for quality control of Yixintong pills.

Apigenin ; analysis ; Chromatography, High Pressure Liquid ; Crataegus ; chemistry ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; Plant Leaves ; chemistry ; Plants, Medicinal ; chemistry ; Quality Control

OBJECTIVETo compare and analyze the organic acids level in fruit of Crataegus pinnatifida var. major before and after processing.

METHODThe amount of total organic acids and individual citric acid, malate acid, ursolic acid and oleanolic acid in fruit of C. pinnatifida var. major before and after processing were determined by pH titration and HPLC analysis.

RESULTGood linear relationship between peakarea and amount was noted for 0.28-9.02 microg of malate acid, with a correlation coefficient of 0.9998. Regression equation was Y = 2344.7 + 49309.6 X. Good linear relationships between the logarithm of peak area and amount were noted for 0.348-1.74 microg of usolic acid and 0.498-2.48 microg of oleanolic acid, with a correlation coefficient of 0.9998 in each case. Regression equations were Y = 1.3628 X + 5.9508 and Y = 1.4447 X + 5.8236, respectively.

CONCLUSIONThe lipid-soluble organic acids mostly remain whereas only about 70% of the water-soluble acids remain after processing in fruit of C. pinnatifida var. major.

Citric Acid ; analysis ; Crataegus ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Fruit ; chemistry ; Hot Temperature ; Malates ; analysis ; Oleanolic Acid ; analysis ; Plants, Medicinal ; chemistry ; Technology, Pharmaceutical ; Triterpenes ; analysis

AIM: To study the chemical constituents and bioactivity of the seeds of Crataegus pinnatifida. METHODS: The chemical constituents were isolated and purified by macroporous adsorptive resin D101, silica gel, and ODS column chromatography, and preparative HPLC. Their structures were elucidated on the basis of spectroscopic methods. In addition, the cytotoxic activities of compounds 1-4 were investigated on OPM2 and RPMI-8226 cells. RESULTS: Four compounds were obtained and their structures were identified as (7S, 8S)-4-[2-hydroxy-2-(4-hydroxy-3-methoxyphenyl)-1-(hydroxymethyl)ethoxy]-3, 5-dimethoxybenzaldehyde (1), (+)-balanophonin (2), erythro-guaiacylglycerol-β-coniferyl aldehyde ether (3), buddlenol A (4). CONCLUSION Compound 1 is a novel norlignan, while compounds 1-4 exhibited marginal inhibition on the proliferation of OPM2 and RPMI-8226 cells.
Cell Line ; Cell Proliferation ; drug effects ; Crataegus ; chemistry ; Humans ; Molecular Structure ; Nerve Tissue Proteins ; chemistry ; isolation & purification ; toxicity ; Plant Extracts ; chemistry ; isolation & purification ; toxicity ; Seeds ; chemistry

In order to investigate the mechanism, the correlation between the odor change in Crataegi Fructus stir-fried process and 5-HMF were studied. Required samples were retrieved from Crataegi Fructus stir-fried process. Statistical quality control (SQC) was used to analyze the response values acquired by the electronic nose. At the same time, the content of 5-HMF was detected by high performance liquid chromatography (HPLC). Correlation analysis was used to analyze the relationship between the above two. Experimental results showed that SQC model established by response values of all samples could show the change law of odor in Crataegi Fructus stir-fried process and changes of 5-HMF content was dropped after the first increase. Correlation analysis showed that the odor change in Crataegi Fructus stir-fried process and 5-HMF were significantly correlated (P < 0.05). Sugar degradation reaction and the Maillard reaction may be one of the mechanisms of the odor change in Crataegi Fructus stir-fried process.
Chromatography, High Pressure Liquid ; Crataegus ; chemistry ; Furaldehyde ; analogs & derivatives ; analysis ; Hot Temperature ; Odorants ; analysis ; Plant Extracts ; analysis ; Technology, Pharmaceutical ; methods

In order to study the pesticide residues of the medicinal Crataegi Fructus,this study aims to establish an analysis method for pesticide residues( mainly containing insecticides and fungicides) suitable for the actual situation of medicinal Crataegi Fructus based on the survey of the pesticides of the Crataegi Fructus base,combined with the blind screening results of the LC-ESI-MS/MS pesticide screening platform established by the research team in the early stage. Then,the pesticide residues in medicinal Crataegi Fructus from Shandong,Hebei,Henan,Shanxi,and Liaoning( main cultivation areas) were analyzed. The samples were pretreated by the modified Qu ECh ERS method,i.e.,extracted with acetonitrile-water( 9 ∶1),purified by PSA,C_(18),GCB,silica gel. The detection of pesticides was performed by LC-MS/MS. The ion source was ESI with positive scanning mode,and the linearity of 11 kinds of pesticides in the range of 5-300 μg·kg~(-1) was acceptable( R~2>0. 996 9). All the recoveries of pesticides were within 70. 02%~(-1)12. 0% in the low,medium and high levels,with RSD≤17%. The results showed that the detection rate of carbendazim,chlorpyrifos and difenoconazole is 79%,82%,56%,respectively. Besides,the prohibition pesticide carbofuran were detected in some of the batches,indicating the security risk. This study provides methodological references and basic data for risk assessment of Crataegi Fructus and government regulation.
Chromatography, Liquid ; Crataegus/chemistry* ; Drug Contamination ; Drugs, Chinese Herbal/analysis* ; Pesticide Residues/analysis* ; Surveys and Questionnaires ; Tandem Mass Spectrometry