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OBJECTIVE To investigate the improvement effects and mechanism of imperatorin on cachexia model mice. METHODS Fifteen male C57BL/6J mice were randomly divided into blank control group， model group and imperatorin group， with 5 mice in each group. Except for blank control group， the remaining mice were inoculated with LLC cell suspension subcutaneously on the dorsal surface， and the drug was administered by gavage daily from the 7th day of inoculation. The imperatorin group was gavaged with imperatorin suspension （0.5% sodium carboxymethylcellulose solution as solvent） at 60 mg/kg； blank control group and model group were given an equal volume of 0.5% sodium carboxymethylcellulose solution， for 13 d of continuous administration. During the administration period， food intake and body mass of mice were recorded daily and regularly， tumor long and short diameters were measured every two days， and tumor volume was calculated. The skeletal muscle mass and tumor mass of each group were weighed and the tumor-free body weight was calculated； the pathological changes of skeletal muscle were observed and the cross-sectional area of skeletal muscle fibers was calculated； the phosphorylation levels of signal transduction and activator of transcription 3 （STAT3） （measured as p-STAT3/STAT3 ratio）， muscle atrophy box F gene （MAFbx）， myostatin （Myog）， B-cell lymphoma-2 （Bcl-2）， Bcl-2 associated X protein （Bax）， Caspase3 protein and mRNA expression were all detected. RESULTS Compared with blank control group， body mass and skeletal muscle mass of model group were decreased significantly （P＜0.05）， and reduced food intake， loose arrangement of skeletal muscle， large cell space were observed； the cross-sectional area of skeletal muscle fiber was significantly reduced， while p-STAT3/STAT3 ratio， protein and mRNA expressions of MAFbx， Bax and Caspase3 were somo_amour@163.com increased significantly （P＜0.05）. The protein and mRNA expressions of Myog and Bcl-2 were significantly reduced （P＜ 0.05）. Compared with model group， body weight， tumor-free weight and skeletal muscle weight were increased significantly in imperatorin group （P＜0.05）； food intake increased， while the expressions of tumor weight and volume were decreased significantly （P＜0.05）； the expressions of above proteins and genes were improved significantly （P＜0.05）. CONCLUSIONS Imperatorin can improve the tumor cachexia state， the mechanism of which may be related to the regulation of ubiquitin-proteasome pathway and anti-apoptosis.
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Objective To establish a HPLC fingerprints of Biyuanjing capsules. Methods The column was Agilent SB-C18(4.6mm×250 mm, 5 µm). The mobile phase was acetonitrile-water with gradient elution at a flow rate of 1.0 ml/min. The detection wavelength was 210 nm. The detection time was 80 min. Results The HPLC fingerprints of Biyuanjing capsules were established. Twenty common peaks were confirmed, of which, 15 peaks were belonging to each crude drug and 5 peaks were identified as chemical components. The overall similarity of the fingerprints of 10 batches of samples was above 90% comparing with the control. Conclusion This method can be used for the quality control of Biyuanjing capsules.
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Objective: To establish an HPLC fingerprint of Cnidii Fructus formula granule analysis method for simultaneous determination of six main coumarin components, including osthol, xanthotoxin, xanthotol, bergapten, imperatorin and isopimpinellin, in order to provide reference for the study of the material basis of Cnidii Fructus formula granule. Methods: The method was performed by high performance liquid chromatography with a Waters XBridge C18 (250 mm × 4.6 mm, 5 μm) column and methanol (A)-0.1% acetic acid (B) as the mobile phase for gradient elution. The flow rate was 0.5 mL/min, the injection volume was 10 μL and the column temperature was 40 ℃. The detection wavelength was set at 320 nm. The chromatographic fingerprint evaluation system published by the State Pharmacopoeia Commission (2012 Edition) was used to establish the fingerprint of Cnidii Fructus formula granule, and the content of six main coumarin components was simultaneously determined. Results: The research on the 18 batches of Cnidii Fructus formula granule showed that the fingerprint similarity was greater than 0.992 and 19 common peaks were calibrated with satisfied peak resolution. The content determination results showed that the content of both xanthotoxin and osthol were the main coumarin components in Cnidii Fructus formula granule. According to the methodological investigation, the precision RSD values were all less than 1.6%. The sample was stable within 48 h and this method had good repeatability. The average recovery rates of xanthotol, xanthotoxin, imperatorin, isopimpinellin, bergapten and osthol were 100.69%, 101.03%, 99.48%, 100.88%, 101.27% and 100.35%, respectively. All of these coumarin components’ RSD were less than 2.5%. The six components showed a good linear relationship within a certain concentration range. The results of the content determination of xanthotol, xanthotoxin, isopimpinellin, bergapten, imperatorin and osthol respectively were 8.01-8.29, 2.37-2.63, 4.30-4.61, 4.04-4.40, 3.45-3.90 and 6.02-6.80 mg/g among the 18 batches of the Cnidii Fructus formula granule. Conclusion: The fingerprint method and the determination method of six main coumarin components in the Cnidii Fructus formula granule established in this study are simple, stable, accurate and reliable. This method can be used for the quality control of the Cnidii Fructus formula granule.
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Objective: To study the coumarins and alkaloids from the stems of Clausena lenis. Methods: The chemical constituents from the stems of C. lenis were separated and purified by silica gel, ODS, Sephadex LH-20 gel column chromatographies and preparative HPLC. Their structures were identified by physicochemical properties, spectroscopic analysis, as well as the comparisons with the data reported in literatures. Results: A total of 18 compounds were isolated from the 90% ethanol extract of the stems of C. lenis, which were identified as 6,8-diprenylumbelliferone (1), byakangelicin (2), tert-O-methylheraclenol (3), pabularinone (4), isogosferol (5), heraclenol (6), imperatorin (7), decursinol (8), xanthyletin (9), marmesin (10), skimmianine (11), kokusaginine (12), N-metilatanina (13), clausine Z (14), murrayanine (15), 2-methoxy-1-(3-methyl-buten-1-yl)-9H-carbazole-3-carbaldehyde (16), claulansine I (17) and clausehainanine A (18). Among them, compounds 1-10 were coumarins and 11-18 were alkaloids. Conclusion: All compounds are isolated from C. lenis for the first time, compounds 2, 3 and 8 are separated from the genus Clausena for the first time.
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Objective: To investigate the chemical constituents of the whole plants of Artemisia rupestris. Methods: The chemical constituents were isolated and purified by silica gel, Sephadex LH-20 column chromatography and semi-preparative HPLC. The structures of the isolated compounds were identified by NMR and MS spectroscopic method. Results: Eighteen compounds were isolated and purified, which structures were identified as 2α-(2',4'-hexadiynoyl)-1,6-dioxaspiro [4,5]-deca-3-ene (1), chrysophanol (2), ethyl vanillate (3), methyl linolenate (4), 8,11-octadecadienoic acid methyl ester (5), eicosane coumaric acid ester (6), emodin (7), 2,5-di-tert-butylphenol (8), phellopterin (9), syringic acid (10), 7-methoxycoumarin (11), vanillin (12), imperatorin (13), oroxylin A (14), 5-hydroxy-3,4',6,7-tetramethoxyflavone (15), erucylamide (16), octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoate (17) and 3,5,3',4'-tetrahydroxy-6,7-dimethoxyflavone (18). Conclusion: Compounds 1, 4, 11-14 and 18 are isolated from A. rupestris for the first time, and all the other compounds were isolated from the genus Artemisia for the first time.
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Imperatorin, which is extracted from umbelliferous plants such as Radix Angelicae Dahuricae, Radix Saposhnikoviae and Fructus Cnidii, belongs to furanocoumarins and is especially rich in Radix Angelicae Dahuricae. Research has shown that imperatorin possesses functions of anti-inflammatory, analgesic, antibactrial, antiviral, antiallergic, anti-tumor, reverse drug resistance in tumor cells, interaction with drug metabolizing enzymes, affecting cardiovascular and nervous system effect. It is also one of the standard components in quality control of various analgesics. In recent years, research findings related to imperatorin is increasing fast. A number of patent applications have been approved for the application of imperatorin in the treatment of anti-tumor and cardiovascular diseases. In addition, since the water insolubility of imperatorin affects its bioavailability, most researchers have gradually attached importance to this aspect of research, such as modifying its structure or synthesizing its derivatives. The literatures on the pharmacological effects and mechanisms of imperatorin at home and abroad in recent years were consulted and summarized in this paper. Imperatorin was found not only to display other pharmacological effects like furanocoumarins but also could cure osteoporosis, skin diseases and show photosensitization. Moreover, the mechanism of its action has the effect of multi-pathway and multi-target, but most of the studies have not identified its targets, which still needs further study. Extensive and significant pharmacological effect make imperatorin show a great potential for development of new drugs. This paper reviews the basic properties, the progress on pharmacological effects and mechanisms of imperatorin, proposes the research status and direction of future reseach. Hopes to provide ideas for researchers and beneficial references for the future development and utilization of imperatorin.
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OBJECTIVE：To prepare Imperatorin ultradeformable liposomes gel （IMP-UDLs-Gel），and to evaluate its quality. METHODS：Based on single factor test ，using 12 h accumulative penetration amount （Q12h）as evaluation index ，the proportion of carbomer 940，glycerol and propyl glycol in formulation of IMP-UDLs-Gel were investigated by orthogonal test. The optimal formulation was screened. The quality of IMP-UDLs-Gel prepared with the optimal formulation was evaluated. RESULTS ：The optimal formulation of IMP-UDLs-Gel included carbomer 940 proportion of 1％，glycerol proportion of 15％ and propyl glycol proportion of 10％. Q12 h of IMP-UDLs-Gel was （11.543±0.241）μg/cm2；the appearance was milky white and translucent ；the particle size was （93.13±1.68）nm，PDI was 0.268±0.012，Zeta potential was （－24.96±1.99）mV；pH was 7.32±0.03； viscosity was （45.37±1.27）g·s；steady flow was （0.727±0.002）μg·h/cm2，lag time was （4.358±0.175）h，apparent permeability coefficient was 1.392×10－3 cm/h，and it has good physical and optical stability. CONCLUSIONS ：The preparation method is stable and feasible ，and the prepared IMP-UDLs-Gel has good adhesion ，stability and transdermal property.
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Objective: To develop a new three-dimensional fingerprinting method and its assessing Methods: based on comprehensive two-dimensional liquid chromatography using Niuhuang Shangqing Pills (NSP) as an example. The developed method could offer new method for the quality control of NSP. Methods: In first dimension, the separation was achieved with an Acquity UPLC HSS CYANO column (100 mm × 2.1 mm, 1.8 μm), methanol-0.1% formic acid in water were used as mobile phases, flow rates were 0.1 mL/min. In second dimension, the separation was achieved with a Kinetex Phenyl-Hexyl column (50 mm × 3 mm, 2.6 μm), acetonitrile-0.1% formic acid in water were used as mobile phases, flow rates were 1.5 mL/min, detection wavelength was set at 254 nm, and acquiring frequency was at 12.5 Hz. Column temperature for each dimension was 40 ℃ and volume of loop linking the two dimensions was 100 μL. Three similarity-calculating Methods:, Euclidean Distance, Cosine, and Correlation Coefficient, were employed to assess the similarities among the 21 samples on the market using medians with arithmetic means of peak volumes of the common peaks as control fingerprints. Results: The three-dimensional fingerprints of 21 batches of NSP samples on the market were developed; Eighteen common peaks were assigned and five of them were identified, which were geniposide (1), pulegone (8), baicalin (9), imperatorin (15), and wogonin (16). Conclusion: A three-dimensional fingerprinting method and its assessing Methods: based on comprehensive two-dimensional liquid chromatography using NSP as an example were successfully developed for the first time, suggesting that it is a feasible method for developing fingerprints for Chinese materia medica. This work improves and supplements the traditional liquid-chromatography fingerprints.
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Objective: To optimize the extraction process parameters of seven herbs in Xiaoruzeng Capsules (XC). Methods: The content of paeoniflorin, ferulic acid, hesperidin, imperatorin and ligustilide was determined by HPLC. The extraction rate of five kinds of index components, the dry extract yield of extracted herbs and the fingerprint similarity of extracts were comprehensively evaluated. The orthogonal experiment was carried out to investigate the effects of ethanol concentration, extraction solvent, extraction time and extraction times on the extraction process. The information entropy weighting method was used to determine the objective weight of each index, and the extraction process parameters of seven herbs in XC were optimized. Results: According to the comprehensive scoring results, it was determined that the best extraction process of the preparation was to add six times the amount of 50% ethanol, and decocted two times for 2 h each time. The average score of the three batches of verification scores was 99.72, and the RSD was 0.24%. Conclusion: The preferred process has high extraction rate, with good stability and repeatability, which is suitable for mass production of the preparation.
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Objective: To analyze the quality of Angelicae Dahuricae Radix (ADR) from national drug evaluation sampling, continuously improve and revise the standard determination method, and ensure the safety of public drug use, six index components of ADR medicinal material and decoction pieces were determined by combining HPLC fingerprint chromatography and quantitative analysis of multi-components by single marker (QAMS). Methods: The determination and exploratory study were carried out according to the National Standard. The establishment of steamed Angelicae dahurica HPLC fingerprint, method for multiple assessment of six index components to conduct a methodological survey determination of multi-index component content of 20 batches of Angelicae dahurica tablets, the final determination of the quality of Angelicae dahurica. Result:s A total of 239 batches of ADR were received from 189 enterprises, in which 225 batches were qualified and 14 batches were unqualified. The qualified rate was 94%. A method that determined content of six kinds of coumarin in ADR decoction pieces using imperatorin as control was established, which could solve the problem of difficulty in obtaining control and consuming long determination time. It would better indicate the drug quality. Conclusio:n The method we had established could be used in qualitative and quantitative analysis of oxypeucedanin hydrate, byakangelicin, oxypeucedanin, berapten, imperatorin and isoimperatorin in ADR decoction pieces. Through this random inspection, it is found that there were still some quality problems in ADR decoction pieces. The quality supervision of traditional Chinese medicine should be strengthened further.
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OBJECTIVE: To study the chemical constituents and analgesic activity of the aerial parts of Skimmia multinervia. METHODS: The chemical constituents were isolated by column chromatography packed with MCI and silica gel, respectively, and the structures of the purified compounds were elucidated by NMR and MS analysis. The analgesic activities of the extract, fractions and selected compounds from the aerial parts of S. multinervia were evaluated by using acetic acid-induced writhing test in mice model. RESULTS: The structures of compounds 1-13 are identified as skimmin (1), imperatorin (2), auraptene (3), umbelliferon (4), scopoletin (5), limonin (6), limonexic acid (7), nomilin (8), citrusin (9), taraxerol (10), kanalpin (11), skimmianine (12), and methyl vanillate (13). The extract, ethyl acetate fraction, and alkaloid fraction could reduce the times of mice writhing induced by acetic acid, and the analgesic effect of compound 3, with inhibition rate of 88.18%, was much better than that of the positive control, aspirin. CONCLUSION: Compounds 1-13 are isolated from the plant for the first time, while 7, 9, 11, and 13 are firstly isolated from Skimmia genus. The analgesic activities of S. multinervia and compound 3 are reported for the first time.
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Aim To investigate the antidepressant effect of imperatorin(IMP) and explore its mechanism. Methods The model of depression was established by prenatal stress (PS) on late pregnant mother, then male offspring rats were randomly divided into five groups: control, PS model, fluoxetine group(5 mg • kg"1), IMP( 15, 30 mg • kg"1). Sucrose preference test, forced swimming test, and open field test were used to evaluate the behavioral changes. 5- hydroxytryptamine ( 5-HT ) concentration, serotonin transporters(5-HTT) and 5-HT,A receptor(5-HT,AR) mRNA expression in the hippocampus and frontal cortex were measured using an enzyme-linked immunosorbent assay and real-time PCR. Results Compared with PS group, the percentage of sucrose preference and the number of total crossings, center crossings, rearing, grooming and 5-IIT concentration significantly increased in IMP group(/> <0. 01). The im-mobility time was significantly reduced in IMP group compared with PS group ( P < 0. 01). The 5-HT concentration and 5-HT1A R mRNA expressions of PS offspring rats significantly increased by the administration ofIMP (P<0.05,P<0.01). And, the increased 5- HTT mRNA markedly decreased in IMP group compared with PS group (P < 0. 05 , P < 0. 01 ). Conclusions IMP can obviously improve rat behavior and show anti-depressant effect, which may relate to the 5- HT concentration, 5-HTT and 5-HT,AR mRNA expression in hippocampus and prefrontal cortex.
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Objective:To establish an HPLC gradient elution method for the determination of isoalantolactone,alantolactone,xan-thotoxol,oxypeucedanin,imperatorin and osthole in Kangfu ointment simultaneously. Methods:Isoalantolactone,alantolactone,xan-thotoxol,oxypeucedanin,imperatorin and osthole were determined by HPLC with a chromatographic column of Agilent TC-C18(250 mm ×4.6 mm,5 μm),the mobile phase was methanol-0.1% formic acid solution with gradient elution at a flow rate of 0.9 ml·min-1. The detection wavelengths were 220 nm and 300 nm. The column temperature was 35℃. Results: The linear range of isoalantolac-tone,alantolactone,xanthotoxol,oxypeucedanin,imperatorin and osthole was 6.16-123.20 μg·ml-1,3.78-75.60 μg·ml-1,1.87-37.40 μg·ml-1,4.06-81.20 μg·ml-1,9.27-185.40 μg·ml-1and 13.89-277.80 μg·ml-1,respectively. The correlation coef-ficient was 0.999 4,0.999 8,0.999 6,0.999 5,0.999 9 and 0.999 7, respectively. The average recovery was 98.04% (RSD=1.06%),97.10%(RSD = 1.53%), 96.73% (RSD = 0.90%), 98.92% (RSD = 1.36%), 99.12% (RSD = 0.83%) and 100.27%(RSD=0.58%),respectively. Conclusion:The method is simple and accurate,which can be used to improve the quality standard for Kangfu ointment.
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Objective The HPLC-MS/MS is used to comprehensively monitor the feeding conditions of raw materials in Yuanhu analgesic capsules, and the content of the index components can be detected at the same time. Methods The Inertsil ODS-3 (4.6 mm×250 mm, 5 μm) was used with the column temperature 40 ℃, Flow phase: 0.1% formic acid-acetonitrile; the gradient elution program, active ingredients were separated by HPLC, and the Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode, and reactions ion monitoring mode (MRM) for quantitative analysis were selected. Results Through analysis and contrast of the medicinal materials, reference substance of primary mass spectrogram showed the same characteristic peak, and the proprietary Chinese medicine can be judged by prescription feeding process. The tetrahydroxene and imperatorin had a good linear relationship in 5.08×10-5-30.45×10-5μg (r=0.999 4), 5.02×10-5-30.09×10-5μg (r=0.999 2). Precision test were 0.99% and 1.14%, the recovery rate were 97.02%-99.66%, 97.62%-99.94%. Conclusions The method is simple, accurate and reliable, high sensitive and fast. It is suitable to monitor the feeding condition and quality of yuanhu analgesic capsules.
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Objective To optimize prescription and evaluate the quality of imperatorin lipid microspheres (ILM) by central composite design-response surface methodology (CCD-RSM), therefore to use the mean particle size, particle size distribution (polydispersity index, PDI) and Zeta potential as the primary indicator. Methods Mean particle size, particle size distribution and Zeta potential of lipid microspheres were measured to investigate the effect of the concentration of egg yolk lecithin, poloxamer and percentage of soybean oil in oil phase on the properties of ILM preparation. Mathematic relation between indicator and factor was constructed by binominal fitting. Then the response surface method according to the best mathematical model of evaluation indicators was used to make predictive analysis of the best prescription. Optimized prescription was used to prepare ILM and evaluate its quality. Results Optimized prescription was egg yolk lecithin 1.50 g, F68 0.35 g, and MCT 10 g. All items of optimized prescription were similar to target values. According to the optimized prescription, mean particle size of ILM was (165.00 ± 0.22) nm, particle size distribution was 0.046 ± 0.070, Zeta potential was (−30.30 ± 0.13) mV, encapsulation efficiency was about 90.09%, drug-loading rate was 1.0 mg/mL. Conclusion Due to the better predictability of constructed mathematical model, CCD-RSM can be applied to optimize prescription of lipid microspheres and the optimized ILM meet pharmacy requirements.
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Objective To prepare the reservoir patch of coumarins in Angelicae Dahuricae Radix and investigate its release and transdermal absorption characteristics in vitro. The efficient enhancers were chosen to improve the drug’s permeation rate. Methods The reservoir patch was prepared using hydroxypropyl methylcellulose (HPMC) as medium and ethylene vinyl acetate (EVA) membrane to control the release of drug. The Franz diffusion cells were used and HPLC was used to determine imperatorin content and permeation rate. The content of imperatorin was determined by HPMC. The effect of the gel consumption, the content of coumarins and penetration enhancer on the transdermal flux were investigated by selecting porcine skin as model. The release of the selected patch in vitro was investigated. Results 1% HPMC, 1% coumarins in Angelicae Dahuricae Radix, 1% Isopropyl Myristate (IPM) and 3% Azone were the best permeation of the patch. The permeation rate reached 0.713 μg/(cm2•h). The release mechanisms of the patch in vitro coincided with zero-order kinetic. Conclusion The reservoir patch of coumarins in Angelicae Dahuricae Radix had high transdermal rate and complete in vitro release. It was indicated that the patch could be expected to be an effective transdermal drug delivery system.
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Objective The best combination of nitrogen, phosphorus and potassium and application amount of fertilizer were studied to provide technical support and theoretical basis for rational fertilization in the production of Chuanmingshen violaceum. Methods The effects of N, P and K application on yield and main effective components of C. violaceum were studied by L9(34) orthogonal experiment design. Results Reasonable N, P, and K application could significantly increase the yield of C. violaceum, and was beneficial to the accumulation of total polysaccharides and the content of imperatorin. Among them, the yield of 75.22 kg/hm2 under the combination of N2P1K2 was the highest, the increase rate was 60.67%, the total polysaccharide content was 25.46%, and the content of imperatorin was 0.489 mg/g. The yield of 44.82 kg/hm under the combination of N3P2K2 was the lowest, the total polysaccharide content was 2.40%, and the content of imperatorin was 0.379 mg/g. The effects sequence of N, P, and K fertilizers on the yield of C. violaceum were N > P > K. The nitrogen fertilizer had the most obvious effect on the yield of C. violaceum, followed by phosphate fertilizer, and potassium fertilizer had the worst effect. Conclusion Under the conditions of this experiment, the best combination of fertilization was N2P1K2 or N2P3K1. The optimum amount of fertilization of N, P2O5, and K2O were 1.08, 0.73, and 0.83 kg/hm2, respectively; or 1.08, 1.10, and 0.50 kg/hm2, respectively.
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Objective To explore the therapeutic effect of imperatorin (IMP) in the asthmatic mice model, and study whether its mechanism is related to Nrf2/HO-1 signaling pathway. Methods A total of 50 male BALB/c mice were randomly divided into five groups, namely the control group, the OVA asthma model group, and the IMP low, medium and high dose treatment groups (15, 30, and 60 mg/kg). HE, Masson, and PAS staining were used to observe lung histopathological changes in mice; ELISA was used to detect the contents of IL-4, IL-5, IL-13, IFN-γ, and IgE in the BALF of mice; DHR-123 was used to detect the content of ROS in the mice BALF; The expression levels of protein carbonyl and MDA in lung tissues of mice were measured; The anti-oxidant enzyme kit was used to detect SOD, GSH, and total antioxidant capacity (TAOC) in BALF; immunohistochemical method was used to detect the expression levels of Nrf2 and HO-1 in lung tissues; The contents of Nrf2 and HO-1 in lung tissues were quantitatively analyzed by Western blotting. Results Compared with the model group, IMP reduced the exudation of inflammatory cells, the proliferation of goblet cells, and collagen deposition; IMP reduced the expression of ROS, total IgE, and OVA specific IgE in BALF; IMP decreased the contents of IL-4, IL-5, IL-13, protein carbonyl, and MDA, and increased the content of IFN-γ, SOD, GSH, and TAOC; The results of immunohistochemistry indicated that IMP increased the expression of Nrf2 and HO-1 in lung tissues; Western blotting showed that IMP induced Nrf2 nuclear translocation and the expression of HO-1 at the protein level. Conclusion IMP plays a therapeutic role in asthmatic mice induced by OVA, and its mechanism may be related to the activation of Nrf2/HO-1 pathway.
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Objective To study the chemical constituents from the fresh fruits of Physalis pubescens. Methods Compounds were isolated and purified by repeated column chromatography on silica gel column, Sephadex LH-20 gel column, and preparative HPLC methods. Physicochemical properties and spectroscopic methods were employed for the structure elucidation. Results Twenty compounds were obtained and identified as osthol (1), xanthotoxin (2), isopimpinellin (3), imperatorin (4), (-)-meranzin hydrate (5), auraptenol (6), 1-(4-hydroxy-3,5-dimethoxyphenyl) ethanone (7), 2,5-dimethoxybenzoquinone (8), 2-(4-hydroxyphenyl) acetic acid (9), (S)-methyl 2-hydroxy-2-(4-hydroxyphenyl) acetate (10), pyrocatechol 1-O-β-D-glucopyranoside (11), benzyl β-D-glucopyranosyl (1→6)-β-D-glucopyranoside (12), 2-phenylethyl-O-β-D-glucopyranoside (13), p-hydroxybenzene propanoic acid (14), 3,4-dihydroxybenzene propionic acid (15), (1-O-p-coumaroyl)-(6-O-β-glucosyl)-β-glucoside (16), 1-O-trans-cinnamoyl-β-D- glucopyranosyl-(1→6)-β-D-glucopyranoside (17), N-trans-feruloyltyramine (18), kaempferol 3-O-β-D-glucopyranoside (19), and bergapten (20), respectively. Conclusion Compounds 1-16 are obtained from Physalis genus for the first time.
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OBJECTIVE:To establish a method for simultaneous determination of chlorogenic acid, baicalin and imperatorin in Biyanling tablets. METHODS:HPLC method was adopted. The separation was performed on a Waters SunFire C18 column with mobile phase consisted of methanol-0.20% phosphoric acid(gradient elution)at the flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm and column temperature was 30 ℃. The sample size was 20 μ L. RESULTS:Linear ranges of chlorogenic acid,baicalin and imperatorin were 1.618-16.18 μg/mL,1.624-16.24 μg/mL and 1.762-17.62 μg/mL(r were 0.999 9),respectively. The limits of quantitation were 2.67,2.03,1.87 μg/mL,and the limits of detection were 1.34,1.06, 0.98 μ g/mL,respectively. RSDs of precision,stability and reproducibility tests were all lower than 2.0%. The recoveries were 98.01%-101.80%(RSD＝1.38%,n＝9),98.38%-101.40%(RSD＝1.26%,n＝9)and 98.06%-101.40%(RSD＝1.28%,n＝9), respectively. RSDs of tolerance tests were all lower than 2.0%. CONCLUSIONS:The method is simple,accurate,precise,stable, reproducible and durable. It can be used for simultaneous determination of hlorogenic acid,baicalin and imperatorin in Biyanling tablets.