Study on chemical constituents of Hippocampus trimaculatus Leach / 药学实践杂志

Objective To study the chemical constituents of Hippocampus trimaculatus Leach. Methods After extracted with ethanol, Hippocampus trimaculatus Leach was isolated and purified by silica gel column chromatography, Sephadex LH-20 gel column chromatography, and reversed-phase C18 column chromatography. The structures of compounds were identified by physical and chemical properties, spectral data and literature comparison. Results Eight compounds were isolated from Hippocampus trimaculatus Leach and identified as L-phenylalanine (1), alanine (2), inosine (3), cholesterol (4), N-acetyltyramine (5), uracil (6), D-mannitol (7), tetrodoine (8), respectively. Conclusion Compounds 5, 7, 8 are isolated from Hippocampus trimaculatus Leach for the first time.

Analysis of chemical components of Shenqi tiaoshen formula / 中国药房

OBJECTIVE To analyze chemical components of Shenqi tiaoshen formula （SQTS）. METHODS UPLC-QE-MS method was adopted. The determination was performed on ACQUITY UPLC BEH C18 column with mobile phase consisted of 0.1% formic acid solution-0.1% formic acid acetonitrile solution （gradient elution） at the flow rate of 0.4 mL/min. The column temperature was set at 40 ℃ ， and the sample size was 5 μL. The electrospray ionization source was used to scan positive and negative ions， and the scanning range was m/z 100-1 500. Combined with TCMSP， PubChem and other databases， SQTS active component database was established and the components were identified in combination with relevant literature. RESULTS & CONCLUSIONS Totally 131 chemical components were identified from SQTS， including 23 terpenoids， 22 flavonoids， 21 phenylpropanoids， 12 alkaloids， 11 phenols， 9 amino acid derivatives， 4 fatty acyls， 3 organic acids and others， such as rutin， citrinin， synephrine， cinnamic acid and ginsenoside Rg1，etc. The cracking process of the main components involved the breaking of glycosidic bonds， dehydration， etc.

Structure identification and content analysis of active components in Xiaoyao pills / 药学学报

Xiaoyao pills are a famous traditional Chinese medicine collected in Welfare Pharmacy, which is a classic prescription for treating liver depression and spleen deficiency. However, its composition is complex. In order to better control the quality of Xiaoyao pills, in this study, HPLC-ion-trap time-of-flight mass spectrometry (LC-IT-TOF/MS) was used to identify the main ingredients of Xiaoyao pills, paeoniflorin, albiflorin, glycyrrhizic acid, saikosaponin A and saikosaponin B2. Then a liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for simultaneous determination and quantification of the main compounds. Fragmentation pathways of five active components were obtained. The method was validated. Five active ingredients in Xiaoyao pills had a good linear relationship, and the values of RSD (%) of repeatability were all less than 5%, the recovery ranges were between 90% and 115%, and the values of RSD (%) of each substance were less than 10% after the sample solution is placed for 24 hours. Three batches of Xiaoyao pills (concentrated pellets) and two batches of Xiaoyao pills (water pellets) were determined, the contents of paeoniflorin in concentrated pills were more than 4.0 mg·g-1, and those in water pills were more than 2.5 mg·g-1, which was accordance with Chinese Pharmacopoeia. However, other compounds behave differently. This method has high sensitivity and reliable measurement results, which provides basis for quality control of Xiaoyao pills and material basis for pharmacology research.

Mass spectrometry-guided study on cyclic peptides from sponge Reniochalina sp / 药学实践杂志

Objective To study the cyclic peptides from sponge Reniochalina sp. under the guidance of mass spectrometry. Methods Mass spectrometry-guided procedural separation methods were used to track and isolate the cyclic peptides from the sponge genus Reniochalina. The structures of compounds were elucidated by the determination of physicochemical parameters and comparison of spectroscopic data. The preliminary cytotoxic activity of compounds was assessed by the Cell Counting Kit-8 (CCK-8) method. Results Three cyclic peptides were isolated from the sponge Reniochalina sp. and identified as stylopeptide 1 (1), hymenamide D (2) and axinastatin 2 (3). Compound 1 exhibited cytotoxicity against six human cancer cell lines with IC50 values ranging from 6.09 to 17.26 μmol/L. Conclusion Compound 1 - 3 were isolated from Reniochalina sp. for the first time, and compound 1 was a cytotoxic cyclic heptapeptide.

Study on related substances of TSD-1 — a novel P2Y12 receptor antagonist / 药学学报

For quantitative analysis of related substances in TSD-1 active pharmaceutical ingredient, structures of prepared impurities were confirmed by NMR and UHPLC-MS, and a high performance liquid chromatographic method was established to determine the related substances in TSD-1. The analytical column was an Agilent ZORBAX Eclipe XDB-C8 (250 mm × 4.6 mm, 5 µm). The mobile phase A was 50 mmol·L-1 ammonium acetate solution (adjusted pH to 5.8 with acetic acid) and the mobile phase B was acetonitrile. The whole run was carried out by gradient elution at a flow rate of 1.0 mL·min-1. The detection wavelength was set at 240 nm and the column temperature was 30 ℃. The resolutions among peaks of TSD-1, impurity A, impurity B, TSD-D, and TSD-F were good. The calibration curves (n = 7) of TSD-1, impurity A, impurity B, TSD-D and TSD-F were linear in their respective weight ranges of 0.242-48.4 µg·mL-1 (r = 1.000 0), 0.244-9.75 µg·mL-1 (r = 0.999 9), 0.244-4.80 µg·mL-1 (r = 0.999 9), 0.254-1.02 µg·mL-1 (r = 0.999 9), and 0.247-0.987 µg·mL-1 (r = 0.999 9). The lower limits of quantitation were 0.244, 0.244, 0.254, and 0.247 µg·mL-1 for impurity A, impurity B, TSD-D, and TSD-F, respectively, and the average recovery of each impurity ranged from 99.08% to 103.00% with high accuracy. TSD-D and TSD-F were not detected in the three batches of TSD-1 active pharmaceutical ingredients, and impurity A and impurity B were not detected beyond the limit. The established HPLC method is simple, accurate, and suitable for determination of related substances of TSD-1, which can provide a valuable reference for the subsequent development of TSD-1.

Two cardenolide glycosides from the seed fairs of Asclepias curassavica and their cytotoxic activities / 中国天然药物

Two cardenolide glycosides, corotoxigenin 3-O-[β-D-glucopyranosyl-(1→4)-6-deoxy-β-D-glucopyranoside] (1) and coroglaucigenin 3-O-[β-D-glucopyranosyl-(1→4)-6-deoxy-β-D-glucopyranoside] (2), were isolated from the seed fairs of Asclepias curassavica. The structures of 1-2 were determined based on the combination of the analysis of their MS, NMR spectroscopic data and acid hydrolysis. The inhibitory effects of compounds 1 and 2 on human colorectal carcinoma cells (HCT116), non-small cell lung carcinoma cells (A549) and hepatic cancer cells (SMMC-7721) were evaluated. The results showed that both compounds 1 and 2 significantly inhibited the viability, proliferation, and migration of A549, HCT116 and SMMC-7721 cells, suggesting that compounds 1 and 2 can be applied in the treatment of lung, colon and liver cancers in clinical practice. This study may not only provide a scientific basis for clarifying the active ingredients in A. curassavica, but also help to understand its antitumor activity, which can promote the application of A. curassavica in clinical treatment of various cancers.

Chemical constituents of triterpenoids from Euphorbia resinifera / 中国中药杂志

The combination of normal-phase silica gel column chromatography, octadecyl silica(ODS) column chromatography, semi-preparative high performance liquid chromatography(HPLC), etc. was employed to isolate and purify the chemical components from Euphorbia resinifera, and 7 triterpenoids were separated from the ethanol extract of the medicinal materials. Their structures were identified by various spectroscopy methods as cycloartan-1,24-diene-3-one(1), cycloartan-1,24-diene-3-ol(2), 3β-hydroxy-lanosta-8,24-diene-11-one(3), lnonotusane C(4), eupha-8,24-diene-3β-ol-7,11-dione(5), eupha-24-methylene-8-ene-3β-ol-7,11-dione(6), and eupha-8,24-diene-3β,11β-diol-7-one(7). Compounds 1 and 2 are new compounds, and compound 3 is obtained from nature for the first time.

Analysis of Antitussive Active Ingredients of Asplenium sampsoni / 中国药房

OBJECTIVE：To study chemical constitue nts of Asplenium sampsoni ，and to investigate its antitussive effects preliminarily. METHODS ： The 75％ ethanol extract was isolated from A. sampsoni and purified by silica gel column chromatography. The structures of the compounds were identified by physicochemical properties and spectral data （mass spectrum ， hydrogen spectrum and carbon spectrum ）. Kunming mice were randomly divided into negative control group ，test group （the doses of 7 monomers were 0.12 g/kg），and positive control group （same dose of benproperine phosphate ），with 10 mice in each group. The antitussive effect of each compound was evaluated by the method of inducing cough with concentrated ammonia water. RESULTS：Totally 13 compounds were isolated and identified from ethyl acetate and petroleum ether parts of 75％ ethanol extract of A. sampsoni ，i.e. 4-hydroxy-acetophenone（Ⅰ），4-hydroxy-ethyl phenylacetate （Ⅱ），luteolin（Ⅲ），apigenin（Ⅳ），quercetin （Ⅴ），formononetin（Ⅵ），acacetin（Ⅶ），protocatechuic acid （Ⅷ），isorosmarinoside（Ⅸ），quercetin-3-O-β-D-glucopyranoside （Ⅹ），isorhamnetin-3-O-β-D-glucopyranoside（Ⅺ），methyl palmitate （Ⅻ）and imperatorin （XⅢ）. Luteolin could significantly prolong the cough latency and reduce the times of cough in mice （P＜0.05）. CONCLUSIONS ：Thirteen compounds are isolated from this plant for the first time ；luteolin has certain antitussive effect ，and may be the antitussive active component of the plant.

Analysis of Chemical Constituents as Flavonoids and Coumarins in Radix Ardisiae from Different Sources / 中国药房

OBJECTIVE：To identif y and analyze the flavonoids and coumarins in Radix Ardisiae from different sources. METHODS：UPLC-QE-HF-MS/MS was adopted. The determination was performed on Zorbax Eclipse-C 18 column with mobile phase consisted of acetonitrile- 0.1％ formic acid solution （gradient elution ）at the flow rate of 0.3 mL/min. The column temperature was 30 ℃，and the temperature of injector was 4 ℃. The sample size was 2 µL；ESI source was applied in negative and positive scanning ion mode ，the heater temperature was 325 ℃，the sheath gas pressure was 45 arb，the auxiliary gas pressure was 15 arb，the purge gas pressure was 1 arb，the electrospray voltage was 3.5 kV，the capillary temperature was 330 ℃， S-lens RF level was 55％，scan mode was first-order full sca m/z 100-1 500，data-dependent secondary mass spectrometry scanning （dd-MS2，Top N ＝10），the resolution was 70 000 （first mass spectrometry ） ， 17 500 （secondary mass spectrometry），the collision mode was high-energy collision dissociation. Through retrieving foreign and domestic databases as ChemSpider ，mzCloud，mzVault，PubChem，the structure of the compound was identified on the basis of related literatures and reference data ，and the conten ts were compared. RESULTS & CONCLUSIONS：A total of 47 components were separated from Radix Ardisiae of 3 kinds of sources as Ardisia crenata Sims，A. crispa（Thunb.）A. DC. ，A. crenata Sims var . bicolor （Walk）C. Y. Wu et C. Chen. A total of 17 flavonoids were identified ，including 9 flavonols （quercetin 3-O-rhamnoside-7-O-glucoside， myricetin， rutin， mauritanin， kaempferol， quercetin， isorhamnetin， quercetin，mearnsitrin），3 flavan-3-ols [（-）-epigallocatechin，catechin，epigallocatechin gallate ）2 dihydroflavonoids [fustin ， eriodictyol] and 3 other types [ 3-（2，3-dihydro-benzo[1，4]dioxin-6-yl）-7-hydroxy-2-trifluoromethyl-chromen-4-one，methadone， oriciacridone F] ，10 coumarins {bergenin ，（[ 7-hydroxy-4-methyl-2-oxo-2H-chromen-6-yl）oxy]acetic acid ，[7-（carboxymethoxy）- 4-methyl-2-oxo-2hydroxychromo-3-yl]acetic acid ，4，9-dihydroxy-7H-furo[3，2-g]chromen-7-one，6，7-dihydroxy-4-methylcoumarin， esculetin，fraxetin，7，8-dihydroxy-4-methylcoumarin，4-methylumbelliferyl glucuronide ，scoparone}. Results of content analysis showed that in flavonoids and coumarins ，there were 5 common components in Radix Ardisiae from 3 kinds of sources ，i.e. bergenin（peak 2），[7-（carboxymethoxy）-4-methyl-2-oxo-2-hydroxychromo-3-yl] acetic acid （peak 5），methadone（peak 16）， quercetin（peak 18），oriciacridone F （peak 26）；the contents of common components were significantly different. In addition to 5 common components ，there were 22 different chemical components ，which were compounds corresponding to peaks 1，3，4， 6-15，17，19-25 and 27，respectively. Among them ，compounds corresponding to peaks 3，6，8 and 23 were only found in A. crenata Sims var. bicolor（Walk）C. Y. Wu et C. Chen ；compounds corresponding to peaks 12-15，19 were only found in A. crispa （Thunb.）A. DC. UPLC-QE-HF-MS/MS method can efficiently ，accurately and quickly identify the flavonoids and coumarins in Radix Ardisiae from different sources.

Study on chemical constituents of Wedelia trilobata / 中国中药杂志

A new taraxer-based triterpenoid ester, taraxer-14-en-30-al-3β-O-palmitate(1), was isolated from the whole plant of Wedelia trilobata, along with six known compounds, ent-kaur-16-en-19-oic acid(2), 16α-hydroxy-ent-kauran-19-oic acid(3), tara-xerol(4), β-amyrin(5), 1β-acetoxy-4α, 9α-dihydroxy-6β-isobutyroxyprostatolide(6), and stigmasterol(7). Their structures were elucidated with use of a combination of spectroscopic techniques(IR, HR-ESI-MS, 1 D, 2 D NMR data) and chemical methods.

Identification of impurities in nafamostat mesylate using HPLC-IT-TOF/MS: A series of double-charged ions / 药物分析学报

Nafamostat mesylate is a serine protease inhibitor used in the treatment of acute pancreatitis. The im-purities in nafamostat mesylate, the active pharmaceutical ingredient (API), were profiled via high performance liquid chromatography tandem ion trap coupled with time-of-flight mass spectrometer (HPLC-IT-TOF/MS). The chromatography was performed on an ACE-3 C18 column (200 mm × 4.6 mm, 3μm) using methanol and 0.1％ formic acid in purified water as mobile phase at a flow rate of 1.0 mL/min. The ions were detected by IT-TOF/MS with a full-scan mass analysis from m/z 100 to 800. In total, eleven impurities were detected in nafamostat mesylate API. The impurity profile was estimated based on the HPLC-IT-TOF/MS data, including accurate masses, MSn fingerprints of fragmentation pathways and a series of double-charged ions. Finally, seven impurities were identified and reported for the first time. The results will provide technical support for the quality control and clinical safety of nafamostat mesylate.

Identification of amino alcohols related substances of atenolol by LC-Q-TOF/MS / 中国药科大学学报

@#To identify the amino alcohols related substances in atenolol. The related substances in atenolol and its stressed samples were pre-column derivatized with 9-fluorenylmethyl chloroformate. The separation was carried out on an Inertsil ODS-SP column (250 mm×4.6 mm, 5 μm) with linear gradient elution by methanol-ammonium acetate solution as the mobile phases. Electrospray positive ionization high-resolution Q-TOF/MS was used for the determination of the accurate masses and elemental compositions of the parent and fragment ions of these related substance derivatives. The structures of all the detected substances were identified by spectral analysis and synthetic analysis. Under the established conditions, atenolol and its amino alcohols related substances were well separated, and a total of 14 impurity peaks were detected and identified, of which 12 were related substances and 2 were derivatization reaction by-products. The established LC-MS method provides a reference for the examination and quality control of atenolol related substances.

Analysis of Flavonoids Chemical Components in Waste Material during Industrialization of Pueraria thomsonii Resources / 中国药房

OBJECTIVE：To study the composition and contents of flavonoids chemical components in waste material during industrialization of Pueraria thomsonii resources，and to provide reference for comprehensive development and reasonable utilization of the variety. METHODS ：Using“No. 2 Gange”of P. thomsonii from Jiangxi as objects ，UPLC-Q-TOF-MS and HPLC method were adopted to detect the components and contents of flavonoids in the root （with or without cortex ），cortex，flower， fibrous root ，stem，head and dregs （with or without cortex ）of P. thomsonii as well as dry matter of industrial wastewater （with or without cortex ）after precipitation of pueraria powder. RESULTS ：The linearity ，precision，repeatability，stability and recovery of the established method for content determination of 7 flavonoids（puerarin，daidzin，iridoxine-7-O-xylose glucoside ，genistin， iridin，daidzein and kakkalide ）were all in line with the requirements. Totally 12 kinds of flavonoids were identified ，among which the flavonoids in the root ，cortex，stem，fibrous root ，head and dregs of P. thomsonii as well as dry matter of industrial wastewater were the same ，mainly were puerarin ，daidzin，genistein，daidzein and malonyl-daidzein. The flower of P. thomsonii mainly included iridoxine- 7-O-xylose glucoside ，genistin，iridin，kakkalide，6″-O-xylosyldaidzein，but the components as puerarin ， daidzin and its aglycone were not be detected. The content of puerarin in the head of P. thomsonii was the highest （5.765％）. The contents of puerarin in root and dregs of P. thomsonii as well as dry matter of industrial waste-water in samples with cortex were all higher than in corresponding peeled sample. CONCLUSIONS ：The waste material from the industrialization of P. thomsonii resources contains a lot of flavonoids with rich species and high content ，and can be used as an important raw material for obtaining flavonoids such as puerarin.

Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS / 中国实验方剂学杂志

Objective::To rapidly characterize and identify the components of Siwei Tumuxiang San by using high performance liquid chromatography tandem quadrupole-electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q-Exactive-MS/MS). Method::Agilent ZORBAX SB-Aq column (4.6 mm×150 mm, 5 μm) was adopted and 5 mmol·L-1 ammonium acetate+ 0.1% formic acid aqueous solution-acetonitrile were used as mobile phase. According to the separation and structure identification results of chemical components based on the methods of ChemSpider and ChemicalBook database retrieval, a local database of molecular formula, molecular weight, structural formula and MS/MS spectrum information of chemical components in Siwei Tumuxiang San was established. An HPLC-Q-Exactive-MS/MS analysis method was established. The complex compounds of Siwei Tumuxiang San were identified rapidly by using Xcalibar 3.0 software, comparison of reference materials and studies on MS/MS fragment pathways. Result::A total of 110 compounds were identified from the Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS technology, including 3 sesquiterpene compounds from Inulae Radix, 16 alkaloid compunds and 38 isoprene flavonoid compounds from Sophorae Radix flavescentis, 12 triterpenoid saponin compounds, 1 catechin compounds and 4 flavonoid glycoside compounds from Rubus sachalinensis. The fragment pathways of the main types of compounds were summarized. Among them, mass spectrometry information of 31 compounds was reported for the first time. Conclusion::This study can be used to identify the target compounds and non-target compounds in Siwei Tumuxiang San systematically, accurately and quickly, which will lay a foundation for the in vivo analysis and pharmacokinetic study of the formulation.

Chemical Constituents of Ethyl Acetate Extract from Ajuga ovalifolia var. calantha / 中国实验方剂学杂志

Objective:To investigate the chemical constituents from the ethyl acetate extract of 95% ethanol extract from Ajuga ovalifolia var. calantha. Method:A. ovalifolia var. calantha was percolated with 95% ethanol，and the percolate was concentrated under reduced pressure to obtain the extract. The extract was then dispersed with water and extracted with petroleum ether to obtain the petroleum ether extract fraction and water layer. Then ethyl acetate was used to extract the water layer to obtain the ethyl acetate extract fraction. The Compounds from the ethyl acetate extract fraction were isolated and purified by silica gel，Sephadex LH-20，MCI column，ODS column chromatography and semi-preparative high performance liquid chromatography. Their structures were elucidated by interpretation of NMR，ESI-MS and other spectral evidence. Result:17 Compounds were isolated and elucidated as bakkenolide-E（1），loliotide（2），isololiotide（3），（E）-linalool-1-oic acid（4），umbelliferone（5），phillygenin（6），1-（4-hydroxyphenyl）-ethanol（7），（2E）-8-hydroxy-2，6-dimethyl-2-octenoic acid（8），1H-indole-3-carboxylic acid（9），ajugarin I（10），ajugalactone（11），luteolin（12），20-hydroxyecdysone-2-acetate（13），benzyl-4'-hydroxy-benzoyl-3'-O-β-D-glucopyranoside（14），harpagide（15），6-deoxy-8-acetylharpagide（16），and acteoside（17）. Conclusion:Compounds 1，3-4，6-9，14 were isolated from the plants of Ajuga for the first time，and compounds 2，5，10，13，15-16 were isolated from this plant for the first time.

Identification of the related substances of cyclosporin A by LC-MS techniques / 中国药科大学学报

@#To identify the related substances of cyclosporin A by LC-MS techniques, the separation of cyclosporin A and its related substances was carried out on a Hypersil BDS C18(100 mm×4. 6 mm, 2. 4 μm)column with isocratic elution by a mixture of acetonitrile-water-MTBE and formic acid(430 ∶520 ∶50 ∶1)as the mobile phase. Cyclosporin A and its 29 related substances(9 process related and 20 degradants)were well separated under the established conditions. Among them, 13 were listed in EP and the rest 16 were unknown products having not been reported before. Electrospray positive ionization high resolution TOF/MS was used for the determination of the accurate mass and elemental composition of parent ions of all the components, and triple quadrupoles tandem mass was employed for the product mass spectra determination. Thence, the structures of all the 29 detected substances were successfully characterized through spectra elucidation and the fragmentation pathways analysis. The established LC-MS method was successfully employed for the separation and identification of the related substances of cyclosporin A and it is useful for its fermentation processes and quality control.

Isolation and Identification of Chemical Constituents from Ethanol Extract of Camptosorus sibiricus / 中国实验方剂学杂志

Objective:To study the chemical constituents in 95%ethanol extract of the whole plant of Camptosorus sibiricus and determine its antioxidant activity. Method:Compounds were isolated by a combination of various chromato-graphic techniques, including column chromatography over silica gel and Sephadex LH-20 and reversed-phase HPLC. Their structures were identified on the basis of physicochemical properties and spectral data reported in the literature. Result:Eleven compounds were identified as trans-p-coumaric acid (1),trans-p-coumaric acid 4-O-β-D-glucoside (2),cis-p-coumaric acid 4-O-β-D-glucoside (3),(E)-ferulic acid-4-O-β-D-glucoside (4),caffeic acid methyl ester (5),ferulic acid methyl ester (6),syringic acid (7),syringic acid-4-O-β-D-glucopyranoside (8),protocatechualdehyde (9),vanillain (10) and syringaldehyde (11),respectively. Conclusion:Compounds 3-11 are isolated from the genus Camptosorus for the first time. In the in vitro SOD-like activity assays,compounds 7,9-11 show an antioxidant activity with half maximal inhibitory concentration(IC50)values of 16.70,11.70,12.23 and 13.52 μmol·L-1,respectively.

Separation Identification of Chemical Constituents of Lysimachia capillipes / 中国实验方剂学杂志

Objective:To systemically study the chemical constituents of n-butanol fraction from Lysimachia capillipes. Method:The whole plant of L. capillipes was crushed into power,extracted by 70% methanol,concentrated under reduced pressure,and then its n-butanol extract was obtained by fractional extraction. The compounds from n-butanol fraction were isolated and purified by macroporous resin column chromatography,medium pressure ODS,silica gel,Sephadex LH-20 and preparative HPLC. Their structures were identified on the basis of spectral analysis and comparison with literature data. Result:Fifteen compounds including 6 saponins and 9 flavonoid glycosides were isolated from L. capillipes,and were identified as ascapilliposide B(1) and capilliposide C(2),kaempferol-3-O-β-D-xylopyranosyl(1→3)-[4-O-E-p-coumaroyl-α-L-rhamnopyranosyl(1→2)] [β-D-glucopyranosyl(1→6)]-β-D-galactopyranoside-7-O-α-L-rhamnopyranoside(3),kaempferol-3-O-{[β-D-xylopyranosyl(1→3)-α-L-rhamnopyranosyl(1→6)] [α-L-rhamnopyranosyl(1→2)]}-β-D-3-trans-p-coumaroylgalactopyranoside (4),capilliposide K (5),3β-O-{α-L-rhamnopyranosyl-(1→2)-O-β-D-glucopyranosyl-(1→4)-[O-β-D-glucopyranosyl-(1→2)]-α-L-arabinopyranosyl)}-16α-hydroxyolean-28,13β-olide (6),capilliposide I(7),quercetin-3-O-(2″,6″-di-O-α-rhamnopyranosyl)-β-galactopyranoside(8),kaempferol-3-O-{[β-D-xylopyranosyl(1→3)-α-L-rhamnopyranosyl(1→6)] [α-L-rhamnopyranosyl-(1→2)]}-β-D-galactopyranoside(9),kaempferol-3-O-[2-glucopyranosyl(1→3)rhamnopyranosyl-6-rhamnopyranosyl]-β-D-galactopyranoside(10),kaempferol-3-O-α-L-rhamnopyranosy-(1→2)-[α-L-rhamnopyranosy-(1→6)]-β-D-galactopyranoside(11),capilliposide I(12),kaempferol-3-O-{(β-D-glucopyranosyl-(1→3)-[4-O-(E-p-coumaroyl)]-α-L-rhamnopyranosyl-(1→6)-(β-D-galactopyranoside)}-7-O-α-L-rhamnopyranoside (13),kaempferol-3-O-{[β-D-glucopyranosyl(1→3)]-4-O-(E-p-coumaroyl)}-α-L-rhamnopyranosyl(1→6)-β-D-glucopyranoside-7-O(4-O-acetyl)-α-L-rhamnopyranoside (14),and (3β,20S,23S,24R)-3,20,23,24,25,29-hexahydroxydammaran-21-oic acid-21,23-lactone 3-O-β-D-glucopyranosyl-(1→6)-β-D-gluco-pyranoside(15). Conclusion:The compounds 3,4,6,9,10,13-15 were isolated from this plant for the first time.

Study on Chemical Constituents of Ethanol Extract from Yao Medicine Cissampelopsis spelaeicola / 中国药房

OBJECTIVE： To study the chemical constituents of ethanol extract from Yao medicine Cissampelopsis spelaeicola. METHODS： The petroleum ether， ethyl acetate and n-butanol fraction from 75％ ethanol extract of C. spelaeicola were isolated and purified by silica gel， SephadexLH-20 gel column and AB-8 macroporous resin column， etc. The structures of the compounds were analyzed and identified by physicochemical properties and spectral data （mass spectrometry， hydrogen spectrum， carbon spectrum）. RESULTS & CONCLUSIONS： Twelve compounds were isolated and identified from 75％ ethanol extract of C. spelaeicola. β-sitosterol（Ⅰ） and Stigmasterol（Ⅱ） were isolated from petroleum ether fraction； p-hydroxybenzoic acid（Ⅲ）， β-daucossterol（Ⅳ）， protocatechuic acid（Ⅴ）， 6β-hydroxyeremophi-7（11）-en-12，8β-olide（Ⅵ）， 10β-hydroxyeremophil-7（11）-en-8，12-olide（Ⅶ）， 10β-hydroxyeremophi-7（11），8（9）-dien-8，12-olide（Ⅷ）， Quercetin（Ⅸ）， Hyperin（Ⅹ） and 4α-hydroxy- eudesman-11-ene（Ⅺ） were isolated from ethyl acetate fraction； quercetin-3-O-robinobioside（Ⅻ） was isolated from n-butanol fraction. Compounds Ⅰ-Ⅻ are isolated from C. spelaeicola for the first time. The study can lay material foundation for activity stady of C. spelaeicola.

Study on the Chemical Constituents in the Ethyl Acetate Extract of Balanophora involucrate / 中国药房

OBJECTIVE： To study the chemical constituents in the ethyl acetate extract of Balanophora involucrate， and to provide reference for further enriching chemical constituent of the plant and the development and utilization of B. involucrate. METHODS： The whole plant of B. involucrate was extracted with 75％ ethyl alcohol. The extraction was carried out by petroleum ether， dichloromethane， ethyl acetate and n-butyl alcohol in turn. The chemical compounds from ethyl acetate extract part were isolated and purified by silica gel column， gel column and semi-preparative HPLC. The structures were identified on the basis of spectral spectrum （mass spectrum， hydrogen spectrum and carbon spectrum） data and literature reports. RESULTS： Thirteen compounds were isolated from ethyl acetate extract part of B. involucrate， identified respectively as pyracanthoside （1）， 5，7，3′ ，5′ -tetrahydroxyflavanone （2）， naringenin （3）， homoeriodictyol （4）， hesperetin （5）， sakuranetin （6）， eriodyctiol （7）， aureusidin-6-O-β-D-glucopyranoside （8）， penicillic acid （9）， dihydropenicillic acid （10）， 2-methyl-3-foroic acid （11）， 5-hydroxymaltol （12） and 5， 7-dyhydroxy chromone （13）. Most of them were dihydroflavones. Compounds 2 to 13 are isolated from Balanophora genus for the first time. CONCLUSIONS： The study enriched the chemical constituents of the Balanophora genus and lays foundation for quality evaluation of B. involucrate.