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??OBJECTIVE To identify seven species from Umbilicariales and study the chemical constituents, antioxidant and anti-inflammatory activities of crude products from the hot-water extraction. METHODS The seven species from Umbilicariales were identified using ITS sequence analysis, and the seven crude polysaccharides were extracted from the species by water extraction method. RESULTS Umbilicaria esculenta, Umbilicaria yunnana, Dermatocarpon miniatum and Lasallia papulosa were identified, and the main components of crude polysaccharides from the species were carbohydrates. The crude polysaccharides (JUY) from Umbilicaria yunnana of Jiangxi had the best antioxidant ability, it exhibited a higher scavenging activity of superoxide radicals (EC₅₀=0.56 mg??mL^-1) than Vc (EC₅₀=1.67 mg??mL^-1), and the scavenging activity for hydroxyl radicals (EC₅₀=0.53 mg??mL^-1) was comparable to Vc (EC₅₀=0.51 mg??mL^-1). Anti-inflammatory experimental results show that JUY has the best anti-inflammatory effects, and the better inhibitory effect of IL-1?? than dexamethasone (P<0.01). CONCLUSION The species from Umbilicariales of seven different areas were identified as four genera. The crude polysaccharides (JUY) from Umbilicaria yunnana of Jiangxi had the best antioxidant and anti-inflammatory activities.     

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??OBJECTIVE To study the chemical constituents of the total flavonoids from Sophora flavescens and establish a method for simultaneous determination of seven compounds. METHODS The compounds were isolated by chromatography on silica gel and ODS column and their structures were elucidated by spectroscopic analysis. The samples were analyzed on a Dikma C₁₈ column (4.6 mm??250 mm,5 ??m); gradient elution was performed using mobile phase composed of methanol (A)and water (B); the detection was carried out using a photodiode array detector at 280 nm. RESULTS Seven compounds were isolated and their structures were identified as kuratidine (1), sophoraflavanone G (2), kurarinone (3), isoanhydroicaritin (4), isoxanthohumol (5), formononetin (6), and trifolirhizin (7). The calibration curve was linear within 8.70-87.00, 44.25-442.50, 128.10-1 281.00, 9.40-94.00, 48.40-484.00, 14.20-142.00, and 25.70-257.00 ??g??mL^-1 for kuraridine, sophoraflavanone G, kurarinone, isoanhydroicaritin, isoxanthohumol, formononetin, and trifolirhizin, respectively (r>0.999 0), and the extraction recoveries varied from 95% to 105%. CONCLUSION The main chemical components contributing to antibacterial activity of total flavonoids may be sophoraflavanone G, kurarinone, and isoxanthohumol. The method is simple, rapid, accurate, and can be used simultaneously to determine the contents of the seven active ingredients.     

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??OBJECTIVE To determine simultaneously seven ingredients(syringin, hydroxysafflor yellow A, rutin, kaempferol-3-O-rutinoside, anhydrosafflor yellow B, cholic acid and hyodeoxycholic acid)content in Sanchen Pills by quantitative analysis of multi-components by single marker(QAMS). METHODS With hydroxy-safflor yellow A as the indexes,calculated the relative correction factor(RCFs) between other 6 components, and which was used to calculate the content of each component, at the same time the contents of the 6 components were determined by the external standard method, and to compare the two METHODS of the calculation results, to verify the feasibility and accuracy of QAMs method. RESULTS No significant difference between the quantitative RESULTS by QAMS and external standard method was observed in 10 samples of Sanchen Pill. CONCLUSION QAMS can be used as a simple and accurate quantitative quality evaluation method for the determination of a variety of ingredients in Sanchen Pills, which provides a new reference for the quality control of Sanchen pill.     

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??OBJECTIVE To construct a network of active components-effect target of xiangdan injection and the network of protein interaction,to analyze the functions and pathways involved in the targets,and to investigate its mechanism of multicomponent-multitarget-multipathway in the treatment of coronary heart disease. METHODS The main active components in xiangdan injection, such as danshensu, salvianolic acid A, salvianolic acid B, salvianolic acid D, tanshinone ??A, protocatechuic aldehyde,rosmarinic acid,and oxidated nerolidol were used as the research object to predict targets of active components in xiangdan injection on the basis of reverse docking server (PharmMapper),to screen the targets for the treatment of coronary heart disease through the human genome annotation database (GeneCards), to construct active ingredients-target disease network using Cytoscape 3.5.1 software, to construct target protein protein interaction(PPI) network using STRING platform,and to analyze the target GO biological process and KEGG metabolic pathway using biological information annotation database (DAVID). RESULTS Eight pharmacodynamic components of xiangdan injection act on ACE, HSP90AA1, AKT1, NOS3, F2, F7 and other 257 potential targets for coronary heart disease,which mainly related to the 13 signaling pathways and 12 biological processes. CONCLUSION The main active ingredient of xiangdan injection could treat the coronary heart disease by PPAR, complement and coagulation cascades, HIF-1, estrogen signaling pathway, play a role of anti-inflammatory, anticoagulant, anti-hypoxia, anti-apoptosis and regulating hormones.     

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??OBJECTIVE To design and synthesize brain targeting danshensu (DSS) derivatives and study their metabolism in rat plasma and brain homogenate in vitro. METHODS Tetramethylpyrazine and its derivatives were selected as carriers to design the brain targeting danshen suderivatives. Lipid-water partition coefficient (logP), brain blood concentration ratio (BB), and P-glycoprotein affinity of the derivatives were predicted by some calculation softwares and the better compound DT3 was chosen for the next synthesis. The degradation of DT3 and its intermediate DT1 in rat plasma and brain homogenate were measured by HPLC-UV. RESULTS Two danshensu-pyrazine ester derivatives were synthesized, ie DT1 and DT3. A simultaneous determination method of DT3, DT1, and (3,5,6-trimethylpyrazine-2-yl)methanol (TMPM) in rat plasma and brain homogenate was established. The degradation of DT3 in rat plasma and brain homogenate underwent the following processDT3??DT1??the active metabolites of DSS and TMPM.Compared with DT1, the degradation of DT3 in rat plasma slowed down.The half-lives (t_1/2) of TMPM were 1.68 and 1.71 min, respectively. Also,DT3 could quickly release the active metabolitein rat brain homogenate, and the concentration of TMPM showed a steady increase with a t_1/2 of 222.88 min. CONCLUSION The danshensu-pyrazine ester derivative DT3 has an extended t_1/2 in rat plasma, and it can be degraded to active metabolite quickly in rat brain homogenate.     

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??OBJECTIVE To validate the conventional gel filtration chromatography (GFC) method for determination of the polymer impurities in ??-lactam antibiotics and achieve combination of GFC and RP-HPLC system. METHODS The effectiveness of the conventional GFC method was identified by 2D-GFC??LC-TOFMS and the polymer impurities found by GFC were identified by RP-HPLC. RESULTS The polymer impurities found by GFC mainly were degradation impurities and open ??-lactam ring impurities, which could not effectively characterize the sensitizing polymer impurities in cefotiam hydrochloride. CONCLUSION An effective method to characterize the polymer impurities in ??-lactam antibiotics may be established on the basis of online column switching technique which effectively combines the advantages of GFC and the ability of RP-HPLC to identify the special impurities.     

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??OBJECTIVE To evaluate the applicability of UPLC/MS method for the identification test of human serum albumin (HSA) products including plasma derived and recombinant HSA samples.METHODS ACQUITY UPLC with Vion IMS QTof LC/MS system was used combined with on-line HSA sample desalting with ACQUITY UPLC BEH C₁₈ column. The acquired multiply-charged mass spectrum was processed with MaxEnt1 automatic protein deconvolution software in UNIFI, which can transfer the raw mass spectrometry data to zero charge molecular mass or mass distribution of the intact protein.RESULTS Intact protein mass analysis not only provided the accurate mass of HSA, but also provided an overall view of the heterogeneity of HSA and the relative amounts of various forms. From this study, a very specific mass signal ??(66 437??1), which is the theoretical average M_W of human serum albumin?? was obtained from all the six HSA samples. And the characteristic spectra of different samples were also got.CONCLUSION UPLC/MS method has very good specificity and high sensitivity and can distinguish HSA products made by different manufacturers and processes. The total analytical time is 10 min, which is ideal for the QC identification test of HSA products.     

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??OBJECTIVE To establish a micellar electrokinetic chromatography with diode array detection (MEKC-DAD) method for simultaneous determination of seven components including stilbene glucoside, emodin, aloe-emodin, rhein, chrysophanol, physcion, and catechin in Polygoni Multiflori Radix. of different origins and commercial herbs. METHODS Based on the mode of MEKC, an uncoated fused silica capillary (75 ??m ?? 64.5 cm, 56 cm of effective length ) was adopted, and 25 mmol??L^-1 borax-30 mmol??L^-1 SDS-10% acetonitrile (pH 9.60) was selected for the running buffer. The detection wavelength was set at 254 nm. The separation voltage was 25 kV and the column temperature was maintained at 24 ??. The sample was injected at 5 kPa for 5 s. RESULTS The calibration curves of the seven components in Polygoni Multiflori Radix showed good linearity (r??0.999 4). The average recoveries of the method were between 99.164%-101.504%. CONCLUSION The established method is reliable and accurate, and can be used for the quality control of Polygoni Multiflori Radix.
     

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??OBJECTIVE To optimize the extraction and inclusion processes of ginger oleoresin from Zingiberis Rhizoma Recens. METHODS Supercritical carbon dioxide extraction was selected to extract ginger oleoresin from Zingiberis Rhizoma Recens. The extraction condition was optimized by orthogonal experiment. The inclusion method, the ratio of ginger oleoresin to ??-cyclodextrin and inclusion time were studied as factors of inclusion process. RESULTS The optimized extraction technology was as follows: extraction temperature was 50 ??, extraction pressure was 25 MPa, separation pressure was 9 MPa and extraction time was 90 min. The optimal inclusion method was triturating inclusion, with the ratio of ginger oleoresin to ??-cyclodextrin of 1??8 and inclusion time of 60 min. CONCLUSION The optimized technology of extraction and inclusion is stable and feasible, and can be used for the extraction and inclusion of ginger oleoresin.     

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??OBJECTIVE To prepare PLGA magnetic nanoparticles loaded with tetrandrine, heat the nanoparticles by inductive heating system, and study the particle size, morphology and drug release before and after heating. METHODS Co-loaded PLGA NPs were prepared by emulsion solvent diffusion method; the physicochemical and magnetic characteristics of co-loaded PLGA NPs were investigated by DLS, SEM, TEM and VSM; RP-HPLC and ICP-MS analysis were used to measure the tetrandrine and Fe₃O₄ loading and entrapment efficiency. The EASYHEAT system was applied to heat the nanoparticles and further investigate the changes of particle size, morphology and drug release after inductive heating. RESULTS Tetrandrine-loaded PLGA magnetic nanoparticles showed spherical shape with smooth surface and the Fe₃O₄ NPs were homogeneously distributed inside the polymeric nanoparticles; VSM result indicated that the co-loaded PLGA NPs were superparamagnetic; both tetrandrine and Fe₃O₄ showed good loading and entrapment efficiency. After being heated to 45 ??, the diameter of co-loaded PLGA NPs increased; the morphology changed from a spherical shape into a nondefined, irregular shape; arrangement or aggregation of the incorporated Fe₃O₄ NPs were found. In addition, the drug release amount was also increased. CONCLUSION With superparamagnetic property, the tetrandrine loaded-PLGA magnetic nanoparticles can effectively control the drug release behavior by inductive heating.
     

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??OBJECTIVE To study the secondary metabolites of marine-derived fungus Aspergillus fumigatus YK-7. METHODS The compounds were isolated by several column chromatographic techniques, including silica gel, ODS, Sephadex LH-20 column chromatography, and HPLC, and their structures were identified on the basis of physicochemical properties and spectroscopic analysis. Trypan blue and MTT methods were applied for determining the effects of the compounds on proliferation of cancer cells in vitro. RESULTS Ten compounds were obtained, and their structures were identified as pseurotin A (1), pseurotin A₁(2), 14-norpseurotin A (3), FD-838 (4), demethoxyfumitremorgin C (5), 9??-hydroxyverruculogen TR-2 (6), 6-methoxyspirotryprostatin B (7), spiro[5H,10H-dipyrrolo[1,2-a:1??,2??-d]pyrazine-2-(3H),2??-[2H]indole]-3??,5,10(1??H)-trione (8), terezine D (9), and 14-hydroxyterezine D (10). CONCLUSION Compounds 3, 6, 7, 9, and 10 are isolated from marine-derived fungus Aspergillus fumigatus for the first time. Compounds 1-4 exhibite moderate antiproliferative activity against selected cancer cell lines in vitro.     

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??OBJECTIVE To synthesize the derivatives of 8-amino benzofuran[3,2-d]pyrimidine and study their anticancer activities.METHODS The target compounds were synthesized through a series of reactions, and their anticancer activities in vitro were evaluated against COLO205, MCF-7 and K562 cell lines by MTT as assay. RESULTS Nine title compounds were synthesized and confirmed by EI-MS,¹H-NMR and ¹³C-NMR.Compounds 2, 3d and 5c had good inhibition effect against COLO205, MCF-7 and K562 cells.The inhibition rates of compound 5c against COLO205, MCF-7 and K562 cells were 99.58%,78.75% and 98.68% respectively at 10^-4 mol??L^-1. CONCLUSION The anticancer activity of benzofuran[3,2-d] pyrimidine derivatives is worthy of further study.     

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目的 为发现抗菌氟喹诺酮向抗肿瘤活性转化的有效修饰策略。方法 以均三唑为氧氟沙星C-3羧基的等排体、通过缩环合反应设计了C-3噻二唑并均三唑稠杂环目标化合物(5a~5l,6a~6l)。用元素分析和光谱数据确证化合物的结构,用MTT方法评价了目标化合物对体外培养的SMMC-7721、Capan-1和HL60 3种癌细胞株的抗增值活性。结果 合成了12个新型结构的C-3稠杂环目标化合物,体外抗肿瘤活性强于母体1和相应中间体硫醚酮5的活性,但弱于硫醚酮缩氨基硫脲化合物6的活性。结论 C-3稠杂环等排体的结构修饰值得进一步研究。     

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??OBJECTIVE To synthesize 5-substituted indole-3-deoxypodophyllotoxin derivatives and study their antitumor activity. METHODS The target compounds were synthesized through a series of reactions and their anti-tumor activity in vitro were evaluated against Hela, K562 and K562/A02 cell lines by MTT as assay. RESULTS Ten target compounds were synthesized and confirmed by ¹H-NMR, ¹³C-NMR, and HR-ESI-MS. All the target compounds had different degrees of cytotoxic activity in vitro. Most of the compounds had significant anti-MDR activity in vitro. CONCLUSION 5-Substituted indole-3-deoxypodophyllotoxin derivatives have good antitumor activity and worth of further study.     

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??OBJECTIVE To research the effect of new L-phenylalanine derivatives on acetylcholinesterase(AChE) activity. METHODS New L-phenylalanine derivatives were synthesized from substituted 2-bromo-1-acetophenones by four steps reaction, and their inhibitory activities on AChE were measured by Ellman method in vitro. RESULTS The evaluation results showed that most derivatives possessed AChE inhibitory effect and the activity of compound 8b was the most potent with an IC₅₀ value of 8.73??10^-6 mol??L^-1, which was more potent than that of rivastigmine; moreover, compound 8b had no inhibitory activities to BuChE. CONCLUSION The inhibitory activities of new L-phenylalanine derivatives on acetylcholinesterase are worth studying further.
     

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??OBJECTIVE To investigate the effect of 1-cyclopropyl-6-fluoro-7-(piperazin-1-yl)-3-[5-benzylsulfanyl-4-(3,4,5-trimethoxybenzylidene) amino-4H-1,2,4-triazol-3-yl]-quinolin-4(1H)-one (M27) on apoposis in hepatocarcinoma SMMC-7721 cells in vitro. METHODS SMMC-7721 cells, colon adenocarcinoma cells(HCT-116)and leukemia cell line JURKET were treated by M27 with different concentrations for different time in vitro, the inhibitory effect of M27 and its precursor ciprofloxacin on the cell proliferation were examined by MTT assay. Cell apoptosis was determined by Hoechst 33258 fluorescence staining and TUNEL assay. The effect of M27 on topoisomerase ?? activity was measured using agarose gel electrophoresis by Plasmid pBR322 DNA as the substrate. Mitochondrial membrane potential(????m)was measured by high content screening imaging system. The p53,Caspase-9,Caspase-3,Caspase-8,Bcl-2,Bax and cytochrome C protein expressions were determined by Western blotting analysis. RESULTS The proliferation of the cancer cells was inhibited by M27 at 10-60 ??mol??L^-1 in time-and dose-dependent manner. Ciprofloxacin showed weak cytotoxicity against SMMC-7721 cell. SMMC-7721 cells treated by M27 with different concentrations for 24 h increased the percentage of apoptosis cells obviously (P<0.05) with a decrease in the mitochondrial membrane potential. Compared with control group, M27 influenced obviously DNA topoisomerase ?? activity, stimulated DNA cleavage and inhibited DNA reunion mediated by topoisomerase ??. In addition, M27 increased protein expression of p53, Bax, Caspase-8, Caspase-9, Caspase-3, as well as the cleaved activated forms of Caspase-9, Caspase-8 and Caspase-3 significantly, whereas the expression of Bcl-2 decreased. There was a significant increase of cytochrome C in the cytosol after 24 h of treatment with M27 and a decrease in the mitochondrial compartment. CONCLUSION M27 as a fluoroquinolone derivative exerted potent anticancer activity through the mechanism of eukaryotic topoisomerase ?? poisoning. The growth inhibition is mainly mediated via apoptosis-associated mitochondrial dysfunction and regulation of Bcl-2 signaling pathways.     

蜘蛛香炮制品的化学成分和抗炎活性研究

目的 研究蜘蛛香炮制品的化学成分及其抗炎活性。方法 采用正相硅胶柱色谱、羟丙基葡聚糖凝胶(Sephadex LH-20)、ODS和高效液相色谱(HPLC)等多种分离材料和方法进行分离纯化,通过理化性质及波谱数据鉴定化合物结构,采用脂多糖(LPS)诱导的RAW264.7细胞体外炎症模型,以总一氧化氮合成酶抑制剂(L-NMMA)作为阳性对照,对化合物进行体外抗炎活性评价。结果 从蜘蛛香炮制品的乙酸乙酯相共分离鉴定了25个化合物,分别为(3S,4R,5S,7S,8S,9S)-3,8-环氧-7-羟基-4,8-二甲基全氢环戊基[c]吡喃(1)、(3S,4S,5S,7S,8S,9S)-3,8-环氧-7-羟基-4,8-二甲基全氢环戊基[c]吡喃(2)、去酰基缬草醛(3)、缬草醛(4)、8-羟基-7′-表松脂醇(5)、(+)-表松脂醇(6)、青刺尖木脂醇(7)、 (7R,8S,7′R,8′S)-5-甲氧基青刺尖木脂醇(8)、(-)-松脂醇(9)、绿原酸(10)、橙皮素(11)、3,8-二羟基-2-甲基色原酮(12)、penicisochroman J(13)、2,5-二(4-羟基-3-甲氧基苯基)-1,4-二烷(14)、4,4′-二羟基-3,3′-二甲氧基-反式-1,2-二苯乙烯(15)、对苯二酚(16)、4-羟基-3-甲氧基苯甲醛(17)、乙酰香草酮(18)、4-羟基-3-甲氧基桂皮醛(19)、2,3-二羟基-1-甲氧基苯(20)、5-羟甲基-2-呋喃甲醛(21)、5-乙酰糠醇(22)、5-[(5-(hydroxymethyl)furan-2-yl)methoxymethoxymethyl]furan-2-carbaldehyde(23)、5-({5-[(5-(hydroxy methyl)furan-2-yl)methoxy(methoxymethyl)]-furan-2-yl} methoxy(methoxymethyl)) furan-2-carbaldehyde(24)和6-羟基-2H-吡喃-3-醛(25)。其中,化合物3,15,16和19均能够显著抑制RAW264.7细胞中脂多糖诱导的一氧化氮生成,且呈显著的剂量依赖性,表现出潜在的抗炎活性。结论 炮制后的蜘蛛香化合物结构类型涉及环烯醚萜及其降解产物、苯丙素、黄酮、色原酮、芳香衍生物和糠醛衍生物等。在炮制过程中,主要是环烯醚萜和单糖的结构发生了变化;化合物 5、6、9~25均为首次从蜘蛛香中分离得到,其中,化合物3,15,16和19具有抗炎活性,半数抑制浓度(IC₅₀)值分别为29.04、10.77、6.37和10.98 μmol·L^-1。     

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??OBJECTIVE To explore the synthesis of novel phenylalanine dipeptide derivatives and their inhibitory effects on tumor cells. METHODS Starting from L-phenylalanine or L-tyrosine, a series of derivatives were synthesized by reaction with chloroacetyl chloride, followed by condensation with L-phenylalaninol or L-phenylalanine methyl ester hydrochloride and nucleophilic substitution reaction with differently substituted phenol.The cell proliferation inhibiting activities of the derivatives were evaluated by thiazolyl blue tetrazolium bromide(MTT)method.RESULTS Some of the target compounds showed certain inhibitory effect for leukemia cell lines K562 and HEL in vitro.Furthermore, the derivatives 3f and 3q had preferably inhibitory effect on K562 cell line prostate cancer PC3 cells in vitro.CONCLUSION Phenylalanine dipeptide derivatives possess good effect on the leukemia and prostate cancer cells and are worth of further research.     

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??OBJECTIVE To study the chemical constituents of the aqueous extract from the aerial part of Sibiraea angustata. METHODS The constituents were isolated by various chromatographic techniques(HP-20 macroporous absorption resin, Sephadex LH-20 gel, Reverse-phase silical gel and PHPLC) and their structures were determined on the basis of physicochemical properties and their spectroscopic data, as well as the literatures. RESULTS Twelve compounds were separated and identified as veratric acid(1),(+)-cycloolivil(2), 3,7-dimethyl-3(E)-6-octadien-5-one-1-O-??-D-glucoside(3), 3,7-dimethyl-3(Z)-6-octadien-5-one-1-O-??-D-glucoside(4), 1-O-??-D-glucopyranosyl(1??2)-??-D-glucopyranosyl-3,7-dimethyl-2(E)-6-heptdiene(5),(7R,8S)-dihydrodehydrodiconiferyl alcohol-9??-O-??-D-glucopyranoside(6),(+)-1-hydroxypinoresinol-1-??-D-glucoside(7), skimmin(8), kaempferol 3-O-??-L-arabinopyranosyl-(1??6)-??-D-galactopyranoside(9), isorhamnetin-3-O-??-D-galactopyranosyl(1??6)-??-D-glucopyranoside(10), isorhamnetin 3-O-??-arabinopyranosyl-(1??6)-??-galactopyranoside(11), and quercetin 3-O-[2''-O-(E)-caffeoyl]-??-L-arabinopyranosyl-(1??6)-??-D-galactopyranoside(12). CONCLUSION All compounds are obtained from the genus of Sibiraea for the first time.