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The original plant species of Fructus Aurantii are multitudinous and complex, and their requirements to the growing environment is strict. In order to clarify the original plant species and geographical distribution of Fructus Aurantii which recorded in the standards and circulated, used in commodity. The national and local standards of Chinese medicinal materials were collected and the original plants of Fructus Aurantii recoded in standards were found. Ten original plant species of Fructus Aurantii (including varieties of cultivars, the same below) were recorded in the Chinese pharmacopoeia and six local standards of Zhejiang, Yunnan and Guizhou etc. The producing areas and commodity in markets of Fructus Aurantii were investigated. The growth environment and geographical distribution of them were analyzed. There are six types of Fructus Aurantii i.e., Fructus Aurantii Chuan, Fructus Aurantii Xiang, Fructus Aurantii Jiang, Fructus Aurantii Qu, Fructus Aurantii Su, Fructus Aurantii Wen, and nineteen species of original plants in the practical commodities. There are four major Fructus Aurantii producing areas: Sichuan Basin, Dongting Lake Plain, Poyang Lake Plain, Jinqu Basin and its surrounding hilly areas. All of them are located in the area of the east longitude 104° to 121° and the northern latitudes 27° to 31°. There is a certain difference between the actual commodity and the standards of medicinal materials. It is suggested that the traditional mainstream types of Fructus Aurantii with fine quality should be accepted into Chinese Pharmacopoeia, and the types with poor quality should be withdrawn from Chinese Pharmacopoeia.
Sujets)
Chine , Citrus , Classification , Médicaments issus de plantes chinoises , Fruit , GéographieRésumé
Aim To investigate the protective effect of Citrus aurantium L. polysaccharides-B(CALB) on ra-diation induced by 60Co γ-ray in mice. Methods The BALB/c mice were randomly divided into blank control group, radiation model group, CALB administration group (high, medium and low dose), and positive control group(black fungus polysaccharide,HP). The mice were administered orally for 30 days. After the last administration for three hours,the survival rates on the 2nd day and the 14th day of the blank control group and the irradiated mice after the single radioac-tive irradiation (7 Gy) with 60Co γ-ray were meas-ured. In addition, DNA content and micronucleus of bone marrow cells, SOD, GSH-Px activities, MDA content in serum, liver and brain tissues in mice, TChE activity in brain tissues and spleen and thymus index of mice were detected after one-time whole body irradiation with 60Co γ-ray (3 Gy). Results Each dose group of CALB could significantly improve the survival rate of irradiated mice,increase the DNA con-tent of mouse bone marrow cells and reduce the number of micronuclei in bone marrow cells. In addition, CALB could also increase the thymus and spleen index and the levels of SOD and GSH-Px in serum,brain and liver tissues of mice,and reduce the content of MDA. Conclusion CALB has protective effect on radiation injury,which can be used for further development and utilization of Fructus aurantii.
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Objective To study compatibility rule of herb-pair in rhubarb after compatibilities with fructus aurantii Immaturus,Chinese goldthread rhizome,moutan cortex,peach seed and kansui radix stir-baked with vinegar, and to observe its anti-inflammation and acute toxicity. Methods Mice were gavaged by 15,30 g?kg-1 rhubarb and rhubarb, rhubarb frutus aurantii immaturus rhizoma coptidis, radix et rhizoma rhei peony, rhubarb, semen persicae and rhubarb extracts from euphorbia kansui, respectively, in the morning and evening once, for 7 d.The effects of five different compatibility of Rhubarb on acute inflammation were observed in the mouse paw swelling induced by carrageenan. The classical method were used to determine acute toxicity of rhubarb and the contents of five different compatibility of rhubarb. Results Compared with the control group, the contents of five different compatibility of rhubarb with high and low dosage groups(30,15 g?kg-1 ) could inhibit the paw edema in mice,reduce NO and MDA production and enhanced activity of SOD in mice inflammatory tissue. The LD50 was not determined. Calculated by crude drug content, the MLD of rhubarb compatibilities with fructus aurantii immaturus, Chinese goldthread rhizome,moutan cortex,peach seed and kansui radix stir-baked with vinegar were 145.33,142.30,117.53,103.45, 113.09,182.36 g?kg-1 respectively, which were respectively equal to 581,569,470,418,452 ,729 times of people, s daily dried medicinal herb dosage. Conclusion The five different herb-pair have anti-inflammation effects after compatibility of Rhubarb, and it got best effects when rhubarb compatibility with kansui radix stir-baked, the next were rhubarb compatibility with Chinese goldthread rhizome and moutan cortex. It was basic security and low toxicity of herb-pair in rhubarb after compatibilities.
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OBJECTIVE: To determine the mass scores of naringin and neohesperidin in Fructus aurantii and Citrus chang-shan-huyou with their processed products and evaluate the quality of Fructus aurantii and Citrus changshan-huyou with their pro-cessed products. METHODS:According to the requirements of Chinese Pharmacopoeia(2010 edition)and Zhejiang Province Tradi-tional Chinese Medicine Preparation Standards (2005 edition),the moisture and ash of F. aurantii and C. changshan-huyou with their processed products were detected. And the contents of naringin and neohesperidin were determined. The ZORBAX SB-C18 column was used with the mobile phase of acetonitrile-water(20∶80,V/V)at the flow rate of 1.0 ml/min. The detection wave-length was set at 283 nm,and the column temperature was 40℃.The samples size was 10μl. RESULTS:The moisture of F. au-rantii and C. changshan-huyou was decreased after processing with no obvious change for ash. The contents of naringin and neohes-peridin were decreased,significantly for F. aurantii,and all consistent with the requirements of Chinese Pharmacopoeia(2010 edi-tion)except F. aurantii. The linear range was 0.028 45-0.284 5μg(r=0.999 7)for naringin and 0.085 9-0.858 6μg(r=0.999 6)for neohesperidin;the RSDs of precision,stability and reproducibility tests were no more than 1.36% and the average recovery was re-spectively 96.45%-100.43%(RSD=1.45%,n=6) and 98.36%-102.00%(RSD=1.26%,n=6). CONCLUSIONS: There was no significant difference in the inspection and determination re-sults in F. aurantii and C. changshan-huyou. It is suggested to adjust the limitation of content determination in the Chinese Pharmacopoeia(2010 edition)and processed standards.
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Objective: To evaluate the quality of commercially available Fructus Aurantii Immaturus (FAI) and Fructus Aurantii FA). Methods: The HPLC fingerprints of FAI and FA were established, and then the quality of FAI and FA purchased from different drugstores was evaluated with multiple data process methods. Results: The quality problem of two batches of FAI were identified. The chemical components of FAI are generally consistent with those of FA. The cluster and principal component analysis methods could be used to distinguish FAI and FA. Conclusion: HPLC fingerprint method can be applied to evaluate the quality of FAI and FA, and to supervise and guide the manufacturers for the purpose of producing qualified products.
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Objective To study the effect of Fructus Aurantii Immaturus Decoction on defecating function of constipated mice.Methods Constipation mice models were induced by Compound Diphenoxylate.Defecating effects of Fructus Aurantii Immaturus on normal and constipation mice were observed.Results Middle and high dose of Fructus Aurantii Immaturus decoction could increase impelling rate of small intestine,shorten the time for the first dark stools(P<0.05 or P<0.01).and add the amount of dark stools within 6 hours(P<0.01).Conclusion Fructus Aurantii Immaturus has the functions of loosening bowel to relieve constipation.
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OBJECTIVE:To establish an HPLC method for simultaneous determination of Naringin,Hesperidin and Neohesperidin in the effective fraction of flavone in Fructus Aurantii Immaturus.METHODS:Hypersil C18 column(250 mm?4.6 mm,5 ?m) was used with the mobile phase consisted of acetonitrile -0.1% phosphoric acid solution(20∶80) at a flow rate of 1.0 mL?min-1,and the detection wavelength was set at 283 nm and the column temperature was maintained at 30 ℃.RESULTS:The calibration curves of Naringin,Hesperidin and Neohesperidin were in good linearity over the ranges of 0.44～2.20 ?g(r=0.999 5),0.025 6～0.128 0 ?g(r=0.999 3),0.54 ～ 2.70 ?g(r=0.999 9),respectively.And the average recoveries for the three constituents were 99.41%,100.33% and 99.69%,respectively with RSD at 1.14%,1.47%,and 1.16%,respectively.CONCLUSION:The method is simple,accurate and reliable,and can be used for the quality control of Fructus Aurantii Immaturus.
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Objective To inspect the quality of Fructus Aurantii Immaturus formula granule. Methods Choose three batch Fructus Aurantii Immaturus to prepare formula granule and decoction. Zobax Extend C18 column was used with acetonitrile-water-phosphoric acid-sodium lauryl sulphate (12∶87∶1∶0.2) as the mobile phase, the detection wavelength was 275 nm. Result There were no differences in elution peak quantity and peak position in the HPLC spectrum of Fructus Aurantii Immaturus formula granule with corresponding cut crude drug and decoction. The relative peak area in the corresponding peak of formula granule had no significant difference with decoction, but had certain differences with cut crude drug. Conclusion HPLC spectrum showed that Fructus Aurantii Immaturus formula granule and decoction had high similarity.
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Objective To study the optimum parameters of the supercritical CO2 fluid extraction of roasted Rhizoma Atractylodis Macrocephalae and roasted Fructus aurantii immaturus,and chemical constituents of extractive matters. Methods The experiment was performed with orthogonal design. Four factors were extractive pressure,temperature,extractive time and the flow rate of CO2. GC-MS was applied for analyzing. Results The optimum condition were obtained:the extractive pressure was 33 MPa,the temperature of extraction was 40 ℃,the extractive time was 60 minutes and the flow rate of CO2 was 27 L/h. The main chemical constituents was gamma-Elemene. Conclusion The method applied to obtain the extractive matters from roasted Rhizoma Atractylodis Macrocephalae and roasted Fructus aurantii immaturus was quickly and efficiently with satisfactory results. It provides foundation for exploration.
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Objective To investigate the different effects of 2 species of Fructus aurantii immaturus on cardiovascular and respiratory system.Methods The extract of 2 species of Fructus aurantii immaturus were administered to anesthetized rats by duodenum and the dosages were 4.2,2.1 g crude drug/kg respectively.After administration,a continuous observation of blood pressure,respiration and ECG effects for 4 hours were performed.Results Compared with the control group,both of Citrus aurantium and Citrus sinesis exerted a transient increase to respiration rate after 20 min administration.No significant impact was observed during the experiment period on the ECG.The influence of Citrus aurantium on blood pressure was more significant.Compared with the control group,the effects of SBP,DBP and MBP reduced was observed in high-dose group of Citrus aurantium after 40,60,80 min administration,and so in low-dose group of Citrus aurantium after 60 min.The impact duration was up to 2 hours or more.However,the antihypertensive effect of Citrus sinesis was not obvious.And the blood pressure lowering effect of Citrus aurantium was superior to Citrus sinesis.Conclusion The 2 species of Fructus aurantii immaturus exert a transient excitatory effect on respiratory system.And the direct effect of them on heart is not obvious.The blood pressure lowering effect of Citrus aurantium is superior to Citrus sinesis.The attention should be given in the clinical usage of Fructus aurantii immaturus.
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Objective To establish a method for determining the content of Naringin and Hesperidin in Zengshi Keli by HPLC. Methods The Kromasil C18 column with acetonitrile-water-phosphoric acid (20∶80∶0.02) as the mobile phase was used. The flow rate was 1.0 mL/min, the detective wavelength was 283 nm, the temperature of column is 35 ℃. Results The calibration curve were linear in the range of 0.178 5～0.892 5 ?g for Naringin and 0.073 68～0.368 4 ?g for Hesperidin (r=0.999 9) respectively. The average recovery was 97.24% (RSD=1.21%) and 96.95% (RSD=1.49%) respectively. Conclusion The method was simple, accurate, reproducible and can be used for quality control of Zengshi Keli.
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Objective To establish a method for the content determination of naringin and hesperidin in Fructus Aurantii Immaturus.Methods HPLC was performed on the Merck-Lichrospher RP-C18 column(4.6?250 mm,5 ?m);CH3CN-H2O(23 ∶77) served as mobile phase and the detection wavelength was at 283 nm,the column temperature at 30 ℃and the flow rate being 1.0 mL/min.Results The content of naringin ranged from 4.65 to 12.50 mg/g and that of hesperidin from 1.60 to 6.75 mg/g.Conclusion This method is simple,sensitive,specific and can be used for the quality control of Fructus Aurantii Immaturus.
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Objective To optimize the extraction process of neohesperidin in Fructus Aurantii Immaturus.Methods The optimum proess was investigated by L9(34) orthogonal design with the content of neohesperidin as the observation index.Results Extraction times were the main factors for neohesperidin extraction.The optimal process condition was as follows:adding 6-fold 70 %ethanol,extracting for 3 times,one hour for each extraction.Conclusion The optimal extraction technology of neohesperidin in Fructus Aurantii Immaturus is stable and reliable.
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Objective To isolate and purify high-purity neohesperidin from Fructus Aurantii extract.Methods Fructus Aurantii extract was treated by macroporous resin and extracted by n-butanol, then concentrated and some solid was precipitated.After crystallizing the precipitate three times, neohesperidin was obtained.The concentration of n-butanol extract was optimized, which was of great importance in the whole preparation.Results The yield of neohesperidin was 48.6% and purity of neohesperidin was up to 98.7% in Fructus Aurantii extract.Conclusion High-purity neohesperidin could be prepared feasibly and economically by proposed method.
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Objective To analyze the chemical components of Fructus Aurantii (FA) and Fructus Aurantii Immaturus (FAI).Methods HPLC-ESI-MS with Surveg mass spectrometer was used in the study.Chromatographic column: Symmetry Shield TM RP_ 18 (150 mm?3.9 mm, 5 ?m) (Waters, Milford, MA, USA); mobile phase: (A) water (0.6% HAc, pH=2.5), (B) methanol. Gradient elutions: 20%- 40% B (0-48 min); 40% B (48-54 min); 40%-55% B (54-60 min); 55%-95% B (60-75 min); 95% B (75-85 min); 95%-20% B (85-90 min).Flow rate and wavelength were 0.7 mL/min and 283 nm at room temperature, respectively.Results Four kinds of flavonoids were identified as naringin, neohesperidin, naringenin, and hesperidin, synephrine was also identified in FA and FAI. Furthermore, the contents of them were determined individually.The results showed that the chemical constituents in FA and FAI were the same but the contents were different.Conclusion HPLC-ESI-MS method can be efficiently used to study FA and FAI.
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Objective To establish HPLC fingerprint for Fructus Aurantii Immaturus.Methods The HPLC method was used with Diamonsil-C18 column (250 mm?4.6 mm,5 ?m),and a mixture liquid of acetonitrile-0.01% NaH2PO4 as mobile phase in a gradient elution.The HPLC fingerprint for 36 batches of Fructus Aurantii Immaturus was studied on their similarity,cluster,and principal components analyses.The common HPLC fingerprint of Fructus Aurantii Immaturus was established,which was studied with principal components analyses.Results Under the selected spectrum condition,the 36 batches of Fructus Aurantii Immaturus were classified into two groups based on the result of similarity,cluster,and principal components analyses.Conclusion This method is reasonable and reliable to the quality control of Fructus Aurantii Immaturus.
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Objective To establish a RP- HPLC method for the determination of naringin and neohesperidin in Fructus Aurantii. Methods The samples were extracted with methyl. The chromatographic conditions were as follows: Hypersil C18 Column( 250 mm? 4.6mm, 5 ? m) , mobile phase of acetonitrile- water(pH=3.0, volume ratio of 19 ∶ 81), detection wavelength at 283 nm, flow rate being 1.0 mL/min and the column temperature at 25 ℃ . Results The calibration curves were linear in the range of 0.156～ 0.934? g for narngin (r=0.9990) and 0.155～ 0.930 ? g for neohesperidin (r=0.9991) . The average recovery of naringin was 101.62 % (RSD=1.91 % ) , and that of nephesoeridin was 103.12 % (RSD=1.22 % ) . Conclusion This method is simple, accurate and reliable for the quality control of Fructus Aurantii.
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Objective To develop a quality standard for Dongfengju oral liq ui d (DOL). Methods Atalantia buxjfolia, Radix Scrophulariae, Fructus Aurantii in DOL was identified by TLC. Results The obtained TLC spots of Atalantia buxj folia, Radix Scrophulariae, Fructus Aurantii in DOL occurred at the correspond ing positions compared to the controls. Conclusion The method is proved to be simple, sensitive, precise and reproducible and can be used for the quality con trol of DOL.
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Objective To study the content difference of naringin in Fructus Aurantii Immaturus of different specifications.Methods HPLC was performed on the Merck- Lichrospher RP-C18(4.6 mm? 250 mm, 5 ? m) with temperature of 35 ℃ .The chromatographic conditions for naringin:the mobile phase consisting of acetonitrile-0.3 % Phosphoric acid(20 ∶ 80), at the flow rate of 1 mL/min, and the detection wavelength at 283 nm. Results The content of naringin increased with the diameter of Fructus Aurantii Immature slices.Conclusion It is suggested that there exists significant differences in intrinsic quality among Fructus Aurantii Immaturus of different specifications.
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AIM: To provide application and identification basis for methanol-extratis of Fructus aurantii by constructing the HPLC-FP. METHODS: The C_(18) column was used with a mobile phase of(A)(0.095%) phosphoric acid acetonitrile-(B)(0.095%) phosphoric acid gradient elution.The flow rate was(1.0) mL/min.The wavelength of detecter was set at 330 nm.Naringin was reference standard. RESULTS: By cluster analysis,the eighteen kinds of Fructus aurantii samples were classified as four clusters: the superior in producing area,the ordinary in producing area,the ordinary and the inferior.By similarity calculation,the similarity of the superior in producing area and the ordinary in producing area were(0.9)～(1.0),and the ordinary and the inferior were less than(0.9). CONCLUSION: The HPLC-FP of Fructus aurantii has been established.The method can be used to identify and evaluate the quality of Fructus aurantii.