白益母草中酚苷类化合物的分离鉴定及其体外抗氧化活性评价

目的 分离鉴定白益母草中抗氧化活性成分。方法 采用常规回流提取法先以二氯甲烷对白益母草脱脂，然后药渣用乙酸乙酯提取得到其提取物。乙酸乙酯提取物利用硅胶、葡聚糖凝胶柱色谱及HPLC进行分离，分离得到化合物经波谱学数据分析，确定其结构式。同时，利用1，1-二苯基-2-三硝基苯肼（DPPH）法测定分离得到化合物的抗氧化活性。结果 从白益母草乙酸乙酯提取物中分离得到4个酚苷类化合物，分别为毛蕊花苷（1），5，7，4''-三羟基黄酮-7-O-（6″-O-[E]-香豆酰基）-β-葡萄糖苷（2），5，7，4''-三羟基黄酮-7-O-（6″-O-[E]-咖啡酰基）-β-葡萄糖苷（3）和5，7，4''-三羟基黄酮-7-O-（6″-O-[E]-二香豆酰基）-β-葡萄糖苷（4）。化合物1~4表现出较好的抗氧化活性，其EC₅₀平均值分别为（19.5±1.81），（26.2±3.4），（22.9±2.7），（24.4±3.1）。结论 化合物1~4均为首次从该药材中分离得到，可作为天然抗氧化剂。     

百蕊草亲水性化学成分研究

目的 对百蕊草中亲水性化学成分进行研究。方法 采用硅胶柱色谱、SephadexLH-20凝胶柱色谱等分离手段,对百蕊草水提取物经AB-8大孔树脂吸附,50%乙醇洗脱的亲水性组分（TT50）进行分离纯化,应用核磁共振波谱分析、结合文献报道鉴定化合物结构。结果 从TT50中分离纯化得到6个化合物,分别鉴定为：山奈酚（1）,紫云英苷（2）,山奈酚-3,7-二-O-β-D-吡喃葡萄糖苷（3）,山奈酚-3-O-L-吡喃鼠李糖基（1→2）-β-D-吡喃葡萄糖苷（4）,山奈酚-3-O-L-吡喃鼠李糖基（1→2）-［6-O-乙酰基］-β-D-吡喃葡萄糖苷（5）,芸香苷（6）。结论 TT50中主要成分为以山奈酚为母核的黄酮苷类化合物,化合物4、5为首次从百蕊草中分离得到。     

平消胶囊联合左甲状腺素钠治疗结节性甲状腺肿的临床研究

目的 对狭叶薰衣草Lavandula angustifolia中的木脂素类化合物进行研究。方法 运用RP-HPLC、TLC、硅胶、凝胶、MCI-gel树脂等方法进行分离纯化,并根据理化性质和波谱数据鉴定化合物的结构。结果 从狭叶薰衣草中分离得到11个木脂素类化合物,分别鉴定为松脂醇（1）、丁香树脂醇（2）、fraxiresinol-4''-O-β-D-glucopyranoside（3）、syringaresinol-4''-O-β-D-glucopyranoside（4）、8-hydroxypinoresinol-4-O-β-D-glucopyranoside（5）、rel-（2α,3β）-7-O-methylcedrusin（6）、落叶松脂醇-4''-O-β-D-葡萄糖苷（7）、（2S,3R）-2,3-dihydro-2-（4-hydroxy-3-methoxyphenyl）-3-hydroxymethyl-7-methoxybenzofuran-5-（trans） propen-1-ol-3-O-β-glucoside（8）、（7S,8R）-dihydrodehydrodiconiferyl alcohol-9-β-D-glucopyranoside（9）、（7R,8R）-7,8-dihydro-9''-hydroxyl-3''-methoxyl-8-hydroxymethyl-7-（4-hydroxy-3-methoxyphenyl）-1''-benzofuranpropanol-9''-O-β-D-glucopyranoside（10）、（E）-3-（（2S,3S）-2-（4-hydroxy-3-methoxyphenyl）-3-hydroxymethyl-7-methoxy-2,3-dihydrobenzofuran-5-yl） allyl-2-hydroxyacetate（11）。结论 11个化合物均首次从狭叶薰衣草中分离得到。     

消乳散结胶囊联合他莫昔芬治疗乳腺增生症的疗效观察

目的 研究瑞香狼毒Stellera chamaejasme花中黄酮和木脂素类化学成分及其抗氧化活性,分析构效关系。方法 利用大孔吸附树脂、正反相硅胶、Sephadex LH-20等色谱分离材料,通过柱色谱和高效液相色谱等分离方法进行分离纯化,运用核磁共振（NMR）、质谱（MS）等波谱技术鉴定化合物结构,并采用FRAP法、DPPH法和ABTS法对分离得到的化合物进行体外抗氧化活性测试。结果 从瑞香狼毒花甲醇提取物中分离鉴定了12个化合物,分别鉴定为艾黄素（1）、槲皮素（2）、isoscutellarein-8-O-β-D-glucuronopyranoside（3）、槲皮素-3-O-β-D-葡萄糖苷（4）、紫云英苷（5）、hypolaetin-8-O-β-D-glucuronopyranoside（6）、kaempferol 3-O-β-D-glucopyranosyl-（1→2）-O-α-L-xylopyranoside（7）、rel-（3R,3''S,4R,4''S）-3,3'',4,4''-tetrahydro-6,6''-dimethoxy[3,3''-bi-2H-benzopyran]-4,4''-diol（8）、马台树脂醇（9）、乌拉尔醇（10）、环黄芪醇（11）、松脂醇（12）。抗氧化活性实验表明,黄酮和木脂素类化合物均显示了较强的抗氧化活性。结论 化合物1、3、5～7和10为首次从该植物中分离得到;化合物2、4、5和10表现出显著的抗氧化活性,其中黄酮类化合物C-3或C-8位连有糖链会降低其抗氧化活性。     

三桠苦枝叶化学成分的分离、鉴定

目的 研究三桠苦[Evodia lepta（Spreng.）Merr.]枝叶的化学成分,为三桠苦的进一步研究奠定物质基础。方法 对三桠苦无水乙醇提取物的乙酸乙酯萃取物采用硅胶柱层析分离纯化,得到单体化合物,经波谱分析鉴定其化合物结构。结果 从三桠苦乙酸乙酯萃取物中分离得到6个单体化合物,分别为异吴茱萸酮酚（化合物1）、异吴茱萸酮酚甲醚（化合物2）、3,5-二羟基-4-乙氧基-6-乙酰基-7-甲氧基-2,2-二甲基苯并二氢吡喃（化合物3）、（cis）-3,4,5-三羟基-6-乙酰基-7-甲氧基-2,2-二甲基色烷（化合物4）和（trans）-3,4-二羟基-5-甲氧基-6-乙酰基-7-甲氧基-2,2-二甲基色烷（化合物5）和对羟基苯甲酸丁酯（化合物6）。结论 化合物1~6均为首次从三桠苦植物的枝叶中分离得到。     

石胆草中黄酮碳苷的分离与结构鉴定石胆草中黄酮碳苷的分离与结构鉴定

目的研究石胆草(Corallodiscus flabellata)的化学成分。方法利用Diaion HP-20,Sephadex LH-20,硅胶柱等色谱技术分离,根据化合物的理化性质和光谱数据鉴定结构。结果从石胆草中分离并鉴定了7个化合物,分别为:5,3′,4′-三羟基-6,7-二甲氧基-8-C-［β-D-木糖-(1→2)］-β-D-葡糖黄酮碳苷(1);5,4′-二羟基-6,7-二甲氧基-8-C-［β-D-木糖-(1→2)］-β-D-葡糖黄酮碳苷(2);5,4′-二羟基-6,7-二甲氧基-8-C-β-D-葡糖黄酮碳苷(3);5,4′-二羟基-6,7-二甲氧基-8-C-［β-D-芹糖-(1→2)］-β-D-葡糖黄酮碳苷(4);3,4-二羟基-苯乙酸乙二醇酯(5);羟基酪醇(6);罗布麻宁(7)。结论化合物1和2为新化合物,其余化合物均系首次从该植物中分离得到。     

泰国产攀援鱼藤的异黄酮苷成分

目的： 对泰国产攀援鱼藤［Derris scandens (Roxb.) Benth］地上部分的化学成分进行分离、鉴定。方法： 采用各种层析色谱技术进行分离。从攀援鱼藤中分离得到2个化合物,用IR,UV,MS,¹HNMR,¹³CNMR,²DNMR光谱鉴定化合物。结果： 经光谱鉴定化合物结构为： 4′-甲氧基－异黄酮-7-O-［α-L-鼠李吡喃糖基(1→6)］-β-D-葡萄吡喃糖苷(I)和4′,8-二甲氧基-异黄酮-7-O-［α-L-鼠李吡喃糖基(1→6)］-β-D-葡萄吡喃糖苷(II), 分别命名为攀援鱼藤苷甲(derriscanoside A)和攀援鱼藤苷乙(derriscanoside B)。结论： 化合物(I), (II)为新的异黄酮苷类化合物。     

复方丹参浸膏中低聚糖成分的分离与结构鉴定

目的 研究复方丹参浸膏中的低聚糖化学成分。方法 采用固相萃取、聚丙烯酰胺凝胶色谱、亲水作用色谱（HILIC）-高效液相色谱（HPLC）-蒸发光散射检测器（ELSD）等技术,对复方丹参浸膏中的低聚糖成分进行分离纯化,并根据理化性质和波谱学手段进行结构鉴定。结果 通过方法优化,成功分离得到了5个低聚糖成分,通过波谱分析鉴定,5个低聚糖成分分别为α-D-吡喃半乳糖-(1→6)-α-D-吡喃半乳糖-(1→6)-α-D-吡喃葡萄糖-(1→2)-α-D-呋喃果糖（1）、α-D-吡喃葡萄糖-(1→2)-β-D-呋喃果糖-(1→1)-α-D-吡喃半乳糖（2）、蔗糖（3）、果糖（4）和葡萄糖（5）。结论 化合物1、2为首次在复方丹参浸膏中分离得到。     

紫茎泽兰中的萜类成分研究

目的 对紫茎泽兰中的萜类成分及其药理活性进行研究。方法 采用D101、HP20大孔树脂、硅胶柱色谱、葡聚糖凝胶色谱、高效液相色谱等多种分离分析手段，MS、¹H-NMR和¹³C-NMR等多种波谱技术以及ECD计算鉴定化合物结构，并采用MTT法对分离得到的单体化合物进行细胞毒活性的筛选。结果 从紫茎泽兰95%乙醇提取物的石油醚和乙酸乙酯萃取部位中分离得到10个化合物，分别鉴定为泽兰酮D (1)、thymoquinol 5-O-β-glucopyranoside (2)、thymoquinol2-O-β-glucopyranoside (3)、2R^*,3S^*-toxol-7-O-β-D-glucopyranoside (4)、6-甲氧基-山柰酚-7-O-β-D-葡萄糖苷(5)、万寿菊素-4’-甲氧基-7-O-β-D-葡萄糖苷(6)、6-hydroxykaempferol-7-O-β-D-glucopyranoside (7)、eupatonriochromene (8)、demethoxyencecalin (9)、encecalin (10)。化合物10对食管癌细胞的IC₅₀值为178.4 μmol·L^-1。结论 其中化合物1为新化合物，化合物6为首次从泽兰属中分离得到，化合物2，3，7为首次从紫茎泽兰中分离得到。化合物10对食管癌细胞Eca-109具有一定的细胞毒活性。     

野葛中的一个新化学成分

应用色谱技术研究豆科植物野葛(Pueraria lobata (Willd.) Ohw)的化学成分，从中分离到5个化合物，通过波谱方法解析它们的结构，分别为：葛根苷D(1)，4′,8-二甲氧基-7-O-β-D-葡糖基异黄酮(2)，二十烷酸(3)，十六烷酸(4)和二十四烷酸-α-甘油酯(5)。化合物1为新化合物，化合物2、3和4为首次从葛根中分离得到。     

Synthesis and evaluation of 2,6-piperidinedione derivatives as potentially novel compounds with analgesic and other CNS activities

New 2,6-piperidinediones 2_a–g and 4_a–d were prepared by initial condensation of aromatic aldehydes or cycloalkanones with cyanoacetamide to give α-cyanocinnamides l_a–g or cycloalkylidenes 3_a,b which underwent Michae1 addition with ethyl cyanoacetate or diethylmalonate. Compounds 4_a–d were alkylated by various alkyl halides to produce the N-alkylated 2,6-piperidinedione derivatives 5_a–m. Some new selected compounds 2_a–c,f, 4_a–d & 5_e,h,j were pharmacologically evaluated for potential anticonvulsant, sedative and analgesic activities. These compounds exhibited significant anticonvulsant and analgesic effects after a single I.P. administration 100 mg/kg b.wt. . On the other hand all the investigated compounds induced hypnotic activity and prolonged the phenobarbital sodium- induced sleep as compared with the control group and the most potent compound was found to be 2_f.     

EFFECT OF POLICOSANOL SUCCESSIVE DOSE INCREASES ON PLATELET AGGREGATION IN HEALTHY VOLUNTEERS

Policosanol is a cholesterol-lowering drug with hypocholesterolemic effects demonstrated in experimental models, healthy volunteers and type II hypercholesterolemic patients. In addition, antiplatelet effects of policosanol have been shown in experimental models and healthy volunteers. The effect of successively increasing doses of policosanol on platelet aggregation was investigated in a randomized, placebo-controlled, double-blind study conducted in 37 healthy volunteers. The volunteers were on a placebo-baseline period (two tablets per day) for 7 days and thereafter they received randomly, under double-blind conditions, placebo or policosanol (10mgday⁻¹) for 7 days. After this period dosage was doubled to 20mgday⁻¹for the next 7 days and then again doubled to 40mgday⁻¹, while the control group received placebo tablets all the time. Platelet aggregation as well as coagulation time was measured at baseline and after each dosing step. Results showed that antiplatelet effects of policosanol were successfully enhanced throughout the study, thus suggesting a dose-dependent relationship. No significant effect was reached during the first dosing period, but significant reductions of epinephrine and ADP-induced platelet aggregation were observed after the second one. Finally, a significant inhibition of platelet aggregation induced by all the agonists was observed at the last dosing step. Coagulation time remained unchanged during the trial.     

NEURAMIDE STIMULATES ADRENOCORTICOTROPIN BUT NOT PROLACTIN RELEASE FROM RAT PITUITARY

Neuramide (NMD), a substance found in crude preparations of porcine stomach extract, is a viral inhibitor that also has putative immunostimulatory effects. The effects of NMD on stress-hormone (ACTH and prolactin—PRL) release were assessed inin vivoandin vitrostudies. In the former, blood levels of corticosterone and PRL were measured in NMD-treated male rats.In vitroexperiments were performed to evaluate the effects of NMD and three of its fractions (obtained with high performance liquid chromatography) on ACTH and PRL release from perfused rat pituitary slices. NMD increased plasma corticosterone levelsin vivoand produced dose-dependent increases inin vitropituitary release of ACTH. No effects on PRL secretion were observedin vivoorin vitro. The stimulatory effects on ACTH release were caused by the NMD fraction with a molecular weight of >5000<10000Da.     

鼻渊净胶囊的HPLC指纹图谱研究

目的 建立鼻渊净胶囊的高效液相色谱（HPLC）指纹图谱。方法 采用Agilent SB-C₁₈（4.6 mm×250 mm,5 μm）色谱柱,乙腈-水为流动相、以1.0 ml/min流速行梯度洗脱,检测波长210 nm,柱温30 ℃,洗脱时间为80 min。采用中药色谱指纹图谱相似度评价系统（2004A版）对检测出色谱进行指纹图谱相似度评价。结果 建立了鼻渊净胶囊的HPLC指纹图谱,确定了20个共有峰,15个峰归属到各药材,其中5个峰确认了化学成分;10批样品的指纹图谱的整体相似度与对照图谱比较,均在90%以上。结论 所建立的鼻渊净胶囊指纹图谱有助于从整体上控制该制剂的质量。     

Investigation of the prevalence of tetQ, tetX and tetX1 genes in Bacteroides strains with elevated tigecycline minimum inhibitory concentrations

In this study, the antibiotic susceptibilities to tigecycline and tetracycline of 35 selected Bacteroides fragilis group strains were determined by Etest, and the presence of tetQ, tetX, tetX1 and ermF genes was investigated by polymerase chain reaction (PCR). tetQ was detected in all 12 B. fragilis group isolates (100%) exhibiting elevated tigecycline minimum inhibitory concentrations (MICs) (≥8 μg/mL) as well as the 8 strains (100%) with a tigecycline MIC of 4 μg/mL, whilst tetX and tetX1 were present in 15% and 75% of these strains, respectively. All of these strains were fully resistant to tetracycline (MIC ≥ 16 μg/mL). On the other hand, amongst the group of strains with tigecycline MICs < 4 μg/mL (15 isolates), tetQ, tetX and tetX1 were found less frequently (73.3%, 13.3% and 46.7%, respectively). All but two strains harbouring the tetQ gene in this group were non-susceptible to tetracycline, with a MIC > 4 μg/mL. These data suggest that in most cases tigecycline overcomes the tetracycline resistance mechanisms frequently observed in Bacteroides strains. However, the presence of tetX and tetX1 genes in some of the strains exhibiting elevated MICs for tigecycline draws attention to the possible development and spread of resistance to this antibiotic agent amongst Bacteroides strains. The common occurrence of ermF, tetX, tetX1 and tetQ genes together predicted the presence of the CTnDOT-like Bacteroides conjugative transposon in this collection of Bacteroides strains.     

INDIRECT PARASYMPATHOMIMETIC ACTIVITY OF THE CLASS III ANTIARRHYTHMIC SUBSTANCE / -SOTALOLIN VITRO: REVERSIBLE INHIBITION OF CHOLINESTERASE ISOENZYMES FROM BLOOD AND THE HUMAN CENTRAL NERVOUS SYSTEM

Inhibitory effects of the class III antiarrhythmic compound / -sotalol on acetylcholinesterase (AChE; EC 3.1.1.7) isoenzymes of both erythrocytes and the human caudate nucleus and on serum cholinesterase (ChE; EC 3.1.1.8) were studiedin vitrousing a spectrophotometric kinetic assay with acetylthiocholine (ASCh) as substrate. Sotalol concentrations in the assays varied from 0.32 to 3.2m . All isoenzymes studied were inhibited by / -sotalol in a reversible and concentration-dependent manner. Double reciprocal plots of the reaction velocity against varying ASCh concentrations revealed that / -sotalol reduced substrate affinity (apparent Michaelis constant, KM, increased) of serum ChE, but did not change the enzyme's maximal rate of ASCh hydrolysis (V_max). Thus, / -sotalol inhibition of serum ChE was of the competitive type (rate constant for reversible competitive inhibition: K_i=0.51m ). In contrast, / sotalol reduced the maximal reaction velocity of the AChE isoenzyme from the central nervous system (caudate nucleus), but had no influence on substrate affinity of the enzyme (K_Mwith ASCh unchanged) indicating purely non-competitive inhibition kinetics (rate constant of reversible non-competitive inhibition: K_i′=0.44m ). / -sotalol inhibition of erythrocyte AChE was of mixed competitive/non-competitive type (K_i=0.31m , K_i′=0.49m ). Non-competitive / -sotalol inhibition of caudate nucleus AChE and the non-competitive component of erythrocyte AChE inhibition cannot be overcome by increased concentrations of the cholinergic transmitter acetylcholine (ACh). Peak / -sotalol plasma levels as described in the literature for both humans (15μ ) and experimental animals (dogs: 18μ ; rats: 260μ ) as well as maximal myocardial concentrations of the substance (dogs: 46μ ; rats: 478μ ) are in the range of about 2% to 100% of the sotalol inhibition rate constants determined in the present paper for cholinesterase isoenzymesin vitro. Thus, / -sotalol inhibition of ACh hydrolysisin vivomay contribute to both the well known antiarrhythmic potential and proarrhythmic side effects of the compound.     

AMELIORIATION OF CHEMICALLY-INDUCED HEPATOCYTE INJURY BY CYCLOSPORINE A

Cyclosporine A, beside its current applications, possesses potential hepatoprotective effects. This study was directed to investigate the effect of Cyclosporine A pretreatment on hepatic injury due to carbon tetrachloride (CCl₄) and -galactosamine. Rats were injected by two successive doses of Cyclosporine A (5mgkg⁻¹day⁻¹). Six hours after the second dose, 1mlkg⁻¹of CCl₄was administered i.p. Effects associated with Cyclosporine A pretreatment were examined by using isolated hepatocytes and hepatocytes that were immobilized and continuously perfused. -Galactosamine (5m ) was added directly to the perfusion medium. After isolation, hepatocytes were examined histologically by light and electron microscopy, immobilized and perfused for further metabolic functional activity evaluation. Cyclosporine A pretreatmentin vivoproduced hepatoameliorative effects of various degrees which were statistically significant as manifested by: (1) an increased trypan blue exclusion after CCl₄; (2) an improved ureagenesis after CCl₄; (3) a reduction in the lipid droplets accumulation in the cytoplasm produced by CCl₄administration; (4) well preserved cytoplasmic organelles as mitochondria, endoplasmic reticulum ER, nuclear chromatin structures that were altered by CCl₄; and (5) an increased hepatocytes survival in the agarose gel matrix, reduction of LD leakage and improvement of ureagenesis after -galactosamine addition to the perfusion medium. The beneficial effect of Cyclosporine A pretreatment in modifying hepatotoxicity of chemical insults merits further studies.     

喙果黑面神化学成分研究

目的研究大戟科植物喙果黑面神(Breynia rostrata Merr.)的化学成分。方法利用硅胶、凝胶等色谱技术分离纯化化学成分,根据化合物的理化性质和光谱数据进行结构鉴定。结果从喙果黑面神的正丁醇萃取部分分离得到4个化合物,分别鉴定为6-O-甲基丙酰基-α-D-吡喃葡糖(6-O-methylpropanoyl-α-D-glucopyranose,1);4″-苯酚基-6-O-甲基丙酰基-β-D-吡喃葡糖苷(4″-phenolic-6-O-methylpropanoyl-β-D-glucopyranoside,2);1-O-没食子酰基-β-D-吡喃葡糖苷(1-O-galloyl-β-D-glucopyranoside,3);熊果苷(arbutin,4)。结论化合物1和2为新化合物,3和4均为首次从该种植物分离得到。     

EFFECTS OF 2-GUANIDINE-4-METHYLQUINAZOLINE ON GASTRIC ACID SECRETION IN RATS

In this study 2-guanidine-4-methylquinazoline (2-GMQ) appeared to decrease basal and stimulated gastric acid secretion, while structurally related compounds as dimethyl- biguanide, cyanoguanidine and 2-cyanoamino-4-methylpyrymidine did not. Thus, there is an antisecretory effect when the biguanide group is associated with a lipophilic structure. The antisecretive effects exerted by 2-GMQ are associated with anti H₂-histamine activity.The anti H₂-histamine nature of the effects of 2-GMQ was confirmed by the capacity of this compound of depressing the chronotropic activity of the isolated guinea pig auricle increased by histamine, as well as relaxant activity in rat uterus contracted by histamine, since both preparations are rich in H₂-histamine receptors.     

栝楼不同药用部位质量控制的研究进展

瓜蒌子、瓜蒌皮、瓜蒌、天花粉来源于栝楼的不同药用部位,4味药材均为常用的大宗药材,现行版《中国药典》对其制定的质量标准过于简单,无法科学合理地控制其质量。本文对瓜蒌子、瓜蒌皮、瓜蒌、天花粉安全性和有效组分的研究进行综述,明确了相关研究存在的问题并针对问题提出建议,为科学全面的药材及饮片标准的制定提供参考依据。