黏萼蝇子草蜕皮甾酮类成分的分离与鉴定

目的对黏萼蝇子草根的化学成分进行研究。方法采用反复硅胶柱色谱、Sephadex LH-20柱色谱和反相半微量制备型高效液相色谱分离纯化,根据ESI-MS、1H-NMR和13C-NMR等谱学数据进行结构鉴定。结果从黏萼蝇子草根的乙醇提取物分离得到5个蜕皮甾酮类化合物,分别鉴定为20-羟基蜕皮激素(20-hydroxyecdysone,1)、1-epi-integristerone A(2)、abutasterone(3)、旌节花甾酮A(stachysterone A,4)和15-羟基旌节花甾酮A(15-hydroxystachysterone A,5);另外得到胡萝卜苷(daucosterol,6)和β-谷甾醇(β-sitosterol,7)2个甾醇类化合物。结论化合物2-5为蝇子草属植物中首次分离的化合物。     

Chemical Composition of Essential Oils from Leaves and Twigs of Pistacia lentiscus,Pistacia lentiscus var. chia,and Pistacia terebinthus from Turkey

The composition of the essential oils from the leaves and twigs of Pistacia lentiscus L., Pistacia lentiscus var. chia (L.), and Pistacia terebinthus L. of Turkish origin were analyzed by gas chromatography/mass spectrometry (GC/MS). Seventy-seven constituents were characterized from the essential oil of P. terebinthus leaves with α-cadinol (6.9%), phytol (5.4%), δ-cadinene (5.1%), α-terpineol (5.0%), and bornyl acetate (4.4%) as major constituents. Germacrene D (10%), β-pinene (7.5%), bornyl acetate (6.0%), α-cubebene (5.9%), and cubebol (5.4%) were found to be the main components among the 61 compounds characterized in the essential oil of P. terebinthus twigs. Forty-six compounds were characterized from the essential oil of P. lentiscus twigs with sabinene (23.2%), α-pinene (19.4%), germacrene D (14.1%), limonene (6.9%), β-phellandrene (6.5%), terpinene-4-ol (5.7%), and β-caryophyllene (5.7%) as the main constituents. Terpinene-4-ol (29.2%), β-caryophyllene (29.2%), and p-cymene (7.1%) were identified as the major components among the 64 compounds characterized in the essential oil of P. lentiscus leaves. Sixty-eight compounds were found on the essential oil of P. lentiscus var. chia leaves with germacrene D (20.1%), myrcene (13.9%), β-caryophyllene (10.8%), and α-terpinyl acetate (4.8%) as the major constituents. Myrcene (27.4%), germacrene D (21.7%), and β-caryophyllene (7.2%) were found to be the main components among 50 compounds characterized in the essential oil of P. lentiscus var. chia twigs.     

Isolation and characterization of microcystins from a River Nile strain of Oscillatoria tenuis Agardh ex Gomont

The River Nile is the major source of drinking water in Egypt, however, increased eutrophication due to agricultural, municipal and industrial runoff has contributed to the growth of toxin producing cyanobacteria. This study describes the isolation and characterization of microcystins (MCYSTs), cyclic heptapeptide hepatotoxins, from a rare strain of Oscillatoria tenuis, isolated from the River Nile at Sohag province in July 1995. The MCYST concentration of laboratory-cultured O. tenuis strain E6 was found to be 0.3 mg/g freeze-dried weight determined by enzyme-linked immunosorbent assay (ELISA). Two microcystins, 1 and 2, were isolated from lyophilized cells using solid phase extraction and reversed-phase high performance liquid chromatography (HPLC). Structures were assigned based upon their amino acid analyses, electrospray ionization mass spectrometry (ESIMS, ESIMS-CID-MS), high resolution fast atom bombardment mass spectrometry, and nuclear magnetic resonance data (¹H and ¹H COSY NMR). Toxin 1 was identified as MCYST-LR, and toxin 2, a new MCYST, as MCYST-LHArg ([ -homoarginine⁴]). Previous studies indicate that Oscillatoria agardhii strains produce demethylated MCYSTs (containing -Asp and/or dehydroalanine). This is the first report of a toxic O. tenuis, strain E6, one which produces a fully methylated MCYST, MCYST-LR and a new -homoarginine containing MCYST, MCYST-LHArg.     

红火麻化学成分的分离与鉴定

目的研究蝎子草属植物红火麻的化学成分。方法利用各种色谱法进行分离纯化,通过理化性质和波谱数据分析进行结构鉴定。结果从红火麻中分离并鉴定了10个化合物,分别为金色酰胺醇乙酸酯(aurantiamide acetate,1)、齐墩果酸(oleanolic acid,2)、2α,3α,19α-三羟基-12-烯-28-乌苏酸(2α,3α,19α-trihydroxyurs-12-en-28-oic,3)、东莨菪素(scopoletin,4)、3-甲氧基-4-羟基苯甲酸(3-methoxy-4-hydroxybenzoic acid,5)、对羟基苯甲酸(p-hydroxybenzoic acid,6)、β-谷甾醇(β-si-tosterol,7)、胡萝卜苷(daucosterol,8)、5-羟甲基糠醛(5-hydroxymethyl furaldehyde,9)、甘露糖(mannose,10)。结论化合物1~10均为首次从红火麻中分离得到,化合物1~6、8~10为首次从蝎子草属植物中分离得到。     

安宫黄体酮母液中两个新化合物的分离与结构鉴定

目的研究药物安宫黄体酮中所含的杂质。方法应用柱色谱方法进行分离和纯化，NMR和MS等波谱方法确定结构。结果从安宫黄体酮母液中分离得到2个化合物。结论化合物1和2为新差向异构体，其结构分别鉴定为：17α-氧乙酰基-2β，6α-二甲基孕甾-4-烯-3，20-二酮；17α-氧乙酰基-2α，6α-二甲基孕甾-4-烯-3，20-二酮。     

牛樟芝水提取物抗过敏作用及其机制研究

目的 研究牛樟芝水提物的抗过敏作用并初步探讨其作用机制。方法 采用大鼠被动皮肤过敏模型、小鼠迟发型超敏模型、小鼠全身皮肤瘙痒模型、小鼠腹腔毛细血管通透性模型,观察牛樟芝水提物在体抗过敏作用。采用体外培养的RBL-2H3肥大细胞,观察牛樟芝水提物对细胞增殖及凋亡的影响,初步探讨其抗过敏反应的作用机制。结果 体内试验中,牛樟芝水提物显著降低大鼠被动皮肤过敏反应,明显降低小鼠耳肿胀度、胸腺指数及脾指数,提高右旋糖酐所致皮肤瘙痒阈值,减少小鼠瘙痒次数,抑制组胺所致血管通透性上升;体外试验中,其剂量相关性的抑制RBL-2H3细胞增殖,促进细胞凋亡。结论 牛樟芝水提取物有一定的抗过敏作用,其机制与促进RBL-2H3细胞凋亡有关。     

Isolation and identification of the toxic peptides from Lophyrotoma zonalis (Pergidae) sawfly larvae

The broad-leaved paper bark tree Melaleuca quinquenervia (Cav) (Myrtaceae) was introduced into Florida (USA) early in this century it has proliferated to such an extent that urgent measures are now required to control it. The sawfly Lophyrotoma zonalis (Pergidae) has been introduced as a possible biological control agent due to its ability to defoliate M. quinquenervia. Because toxic D-amino acid- containing peptides have been isolated from some sawfly species, L. zonalis larvae were processed using the previously reported method for the recovery of these compounds. The toxins lophyrotomin (as the free C-terminal acid) and a mixture of pergidin and Val ⁴-pergidin were isolated at 0.36 and 0.43% yield of the dried larvae, respectively. Both compounds when dosed intraperitoneally to C57/Bl6 male mice were hepatotoxic with lowest lethal doses of 8 and 32 mg/kg, respectively. The pathology of the liver was different for each compound, with the lophyrotomin free acid causing a periportal haemorrhagic necrosis and the pergidin causing a periacinar coagulative necrosis.     

Isolation and identification of antioxidants from Pedilanthus tithymaloides

A bioassay-guided methodology utilizing 2,2-diphenyl-1-picrylhydrazyl (DPPH), the trolox equivalent antioxidant capacity (TEAC), and reducing power assays, as well as an assessment of scavenging properties against O₂^·−, H₂O₂, HOCl, ROO·, ·NO, and ONOO⁻ were used to find the main antioxidant principles of Pedilanthus tithymaloides (Euphorbiaceae), a shrub used in traditional Cuban medicine. The principles were identified as kaempferol 3-O-β-D-glucopyranoside-6′′-(3-hydroxy-3-methylglutarate), quercitrin, isoquercitrin, and scopoletin. The contents of total phenolics and flavonoids were found to be 76.0 ± 4.8 mg of gallic acid equivalents/g extract and 9.8 ± 0.4 mg of rutin equivalents/g extract, respectively.     

金沙槭化学成分的分离与鉴定

目的对金沙槭的化学成分进行系统研究。方法采用硅胶柱色谱、Sephadex LH-20柱色谱、ODS柱色谱、HPLC等手段对金沙槭的乙醇提取物进行分离纯化,并通过化合物理化性质与波谱特征鉴定其结构。结果分离鉴定13个化合物,分别为:槲皮素(quercetin,1)、槲皮素3-O-α-L-阿拉伯糖苷(quercetin 3-O-α-L-arabinoside,2)、槲皮素3-O-α-L-鼠李糖苷(quercetin 3-O-α-L-rhamnoside,3)、槲皮素3-O-β-D-半乳糖苷(quercetin 3-O-β-D-galactopyranoside,4)、山奈酚(kaempferol,5)、山柰酚3-O-α-L-鼠李糖苷(Kaempferol 3-O-α-L-rhamnoside,6)、山奈酚3-O-β-D-葡萄糖苷(kaempferol 3-O-β-D-glucopyranoside,7)、山奈酚3-O-β-D-半乳糖苷(kaempferol 3-O-β-D-galactopyranoside,8)、山奈酚3-O-α-L-阿拉伯糖苷(kaempferol 3-O-α-L-arabinoside,9)、杨梅酮(myricetin,10)、儿茶素(catechins,11)、金线吊乌龟二酮碱A(cepharadione A,12)、巴马汀(palmatine,13)。结论化合物9、12、13为首次从槭属中分离得到。化合物1-13均为首次从该植物中分离得到。     

Screening and isolation of antibiotic resistance inhibitors from herb materials IV-resistance inhibitors fromAnetheum graveolens andAcorus gramineus

The hexane fractions from methanolic extracts ofAnetheum graveolens L. (Umbelliferae) andAcorus gramineus Soland. (Araceae) revealed potent inhibitory activities against the resistance of multi-drug resistantStaphylococcus aureus SA2 when combined with ampicillin (Am) or chloramphenicol (Cm). As active principles, carvone and the liquid mixture containing carvone fromAnetheum graveolens L. and a liquid mixture mainly consisting of benzoic acid phenylmethyl ester (benzyl benzoate) fromAcorus gramineus Soland. were identified. They showed resistance inhibition at the level of 20–50 μg/ml when combined with 100 or 50 μg/ml of Am or Cm, respectively.     

薯蓣属植物化学成分的研究——Ⅱ.叉蕊薯蓣中甾体皂甙的分离和鉴定

从叉蕊薯蓣(D.collettii HooK.f.)根茎的乙醇提取物分离到四个甾体皂甙,根据理化性质、光谱数据,推定化学结构为3-O-(β-D-葡萄吡喃糖)-约莫皂甙元(3-O-(β-D-glucopyranosyl)-yamogenin)[Ⅰ];3-O-[α-L-鼠李吡喃糖(1→4)-β-D-葡萄吡喃糖]-约莫皂甙元(3-O-[α-L-rahmnopyranosyl(1→4)-β-D-glucopyranosyl]-yamogenin)[Ⅱ];3-O-{α-L-鼠李吡喃糖(1→4)-[α-L-鼠李吡喃糖(1→2)]-β-D-葡萄吡喃糖}-约莫皂甙元(3-O-{α-L-rhamnopyranosyl(1→4)-[α-L-rhamnopyranosyl(1→2)]-β-D-glucopranosyl}-yamogenin)[Ⅲ];3-O-{β-D-葡萄吡喃糖(1→3)-[α-L-鼠李吡喃糖(1→2)3-β-D-葡萄吡喃糖}-约莫皂甙元(3-O-{β-D-glucopyranosyl(1→3)-[α-L-rhamnopyranosyl(1→2)]-β-D-glucopyranosyl}-yamogenin)[Ⅳ]。其中Ⅰ为已知物,Ⅱ、Ⅲ、Ⅳ为首次从植物界得到的新甾体皂甙。     

中药牛膝化学成分的分离与鉴定

目的对牛膝(Achyranthes bidentataBl.)的化学成分进行分离、鉴定。方法采用硅胶吸附柱色谱,HPLC等分离手段对牛膝进行分离;利用理化性质、理化反应以及NMR、MS等波谱技术对化合物进行鉴定。结果分离得到5个化合物,分别鉴定为环(酪氨酸-亮氨酸)[cyclo-(-Tyr-Leu),1]、环(亮氨酸-异亮氨酸)[cyclo-(-Leu-Ile),2]、杜鹃花酸(nonanedioic acid,3)、琥珀酸(succinicacid,4)、正丁基-β-D-吡喃果糖苷(n-butyl--βD-fructopyranoside,5)。结论化合物1~3为首次从牛膝中分离得到。首次对化合物1和2进行了碳谱数据归属。     

金钱草中黄酮苷的分离与结构鉴定金钱草中黄酮苷的分离与结构鉴定

目的从金钱草中分离制备标准品。方法用硅胶柱色谱进行分离,通过理化方法及IR,UV,MS,¹HNMR,¹³CNMR,DEPT,HMQC,HMBC等光谱分析确定化合物结构。结果从金钱草中分离得到2个化合物,分别鉴定为鼠李酮酸γ-内酯(I)、山奈酚-3-O-α-L-鼠李糖(1→2)-β-D-木糖苷(II)。结论II为新化合物,命名为金钱草素,I为首次从该属植物中分离得到。     

In vitro and ex vivo activity of new derivatives of acetohydroxyacid synthase inhibitors against Mycobacterium tuberculosis and non-tuberculous mycobacteria

Sulfometuron methyl (SM) is an inhibitor of acetohydroxyacid synthase (AHAS), the first common enzyme in the branched-chain amino acid biosynthetic pathway, and shows activity against Mycobacterium tuberculosis both in vitro and in vivo. To develop AHAS inhibitor derivatives with more potent activity, 100 sulfonylurea analogues were screened for antimycobacterial activity against M. tuberculosis and non-tuberculous mycobacteria (NTM), and then evaluated for intracellular activity using mouse macrophages. Three new compounds with antimycobacterial activity comparable with that of SM were identified. These compounds exhibit significant activity against intracellular M. tuberculosis (including the drug-resistant M. tuberculosis strains), and NTM Mycobacterium abscessus and Mycobacterium kansasii, respectively.     

中药北刘寄奴中黄酮类成分的分离与鉴定

目的研究中药北刘寄奴(Siphonostegia chinensis Benth.)的化学成分。方法采用正相硅胶、反相ODS、Sephadex LH-20等柱色谱及高效液相色谱等手段进行分离纯化,并通过理化性质与光谱分析方法鉴定了化合物的结构。结果从北刘寄奴体积分数为95%的乙醇提取物中分离鉴定了8个黄酮类单体成分,分别为芹菜素(apigenin,1)、芹菜苷(apigentrin,2)、木犀草素(luteolin,3)、木犀草素-7-O-β-D-葡萄糖苷(luteolin-7-O-β-D-glucopyranoside,4)、槲皮素-3-O-β-D-葡萄糖苷(quer-cetin-3-O-β-D-glucopyranoside,5)、槲皮素-3-O-α-L-鼠李糖苷(quercetin-3-O-α-L-rhamnopyranoside,6)、isoscutellarein 8-glucuronide(7)、大豆素(daidzein,8)。结论其中化合物4～8为首次从阴行草属中分离得到。     

薯蓣属植物化学成分的研究——Ⅹ.蜀葵叶薯蓣中甾体皂甙和皂甙元的分离和鉴定

Four components were isolated from acid-treated rhizome of Dioscorea althaeoides Kunth. Their structures were identified as diosgenin (Ⅰ), β-sitosterol (Ⅱ), diosgenin palmitate (Ⅲ) and △^3,5-deoxytigogenin (Ⅳ) on the basis of physical constants and spectral data.Two sparingly soluble steroid saponins were also isolated from this plant Their physicochemical constants showed that one of them is dioscin (Ⅴ) and the other graeillin (Ⅵ).     

火绒草中酚类成分的分离与鉴定

目的对火绒草的化学成分进行分离与鉴定。方法应用硅胶柱色谱、葡聚糖凝胶柱色谱和高效液相制备色谱分离纯化,根据理化性质和波谱数据确定化合物的结构。结果从火绒草中分离得到10个化合物,分别鉴定为咖啡酸乙酯(ethyl caffeate,1)、芹菜素(apigenin,2)、对羟基苯甲酸(P-hydroxybenzoic acid,3)、原儿茶醛(protocatechuic aldehyde,4)、原儿茶酸(protocatechuic acid,5)、咖啡酸(caffeic acid,化合物6)、槲皮素(quercetin,7)、木犀草素(luteolin,8)、对羟基桂皮酸(p-hydroxy cinnamic acid,9)、阿魏酸(ferulic acid,10)。结论化合物1-3、8首次从火绒草中分离得到,化合物1-3为首次从火绒草属植物中分离得到。     

山楂核化学成分的分离与鉴定

目的对山楂(Crataegus pinnatifida Bge.)核中的化学成分进行研究。方法运用硅胶﹑Seph-adex LH-20、ODS柱色谱,制备HPLC,重结晶等分离手段进行分离纯化。根据理化性质及波谱数据鉴定其结构。结果从山楂核体积分数为70%乙醇提取物中分离得到4个化合物,分别鉴定为threo-1-(4-hydroxy-3-methoxyphenyl)-2-[4-(3-hydroxypropyl)-2-methoxyphenoxy]-1,3-propanediol(1)、erythro-1-(4-hydroxy-3-methoxyphenyl)-2-[4-(3-hydroxypropyl)-2-methoxyphenoxy]-1,3-pro-panediol(2)、3-(4-hydroxy-3-methoxyphenyl)-3-methoxypropane-1,2-diol(3)、2-[4-(3-hydroxyprop-yl)-2-methoxyphenoxy]propane-1,3-diol(4)。结论化合物1～4为首次从山楂属植物中分离得到。     

Isolation and identification of chondroitin sulfates from the mud snail

Chondroitin sulfates were isolated from the mud snail. For the quantitative analysis of enzymatic digestion products of isolated chondroitin sulfates, strong anion exchange-high performance liquid chromatography (SAX-HPLC) was performed. By the action of chondroitinase ABC, three unsaturated disaccharides 2-acetamide-2-deoxy-3-O-(β-D-gluco-4-enepyranosyluronic acid)-D-galactose (ΔDi-OS), 2-acetamide-2-deoxy-3-O-(β-D-gluco-4-enepyranosyluronic acid)-6-O-sulfo-D-galactose (ΔDi-6S) and 2-acetamide-2-deoxy-3-O-(β-D-gluco-4-enepyranosyluronic acid)-4-O-sulfo-D-galactose (ΔDi-4S) were produced from the mud snail chondroitin sulfates. The analysis showed that relative proportion of ΔDi-OS/ΔDi-6S/ΔDi-4S was 58.7/3.1/38.2. The immunomodulating activity of chondroitin sulfate was examined by cell proliferation assay and these results suggest that it might be a immunosuppressant.     

西南山茶化学成分的分离与鉴定

目的研究西南山茶叶的化学成分。方法采用硅胶柱色谱、Sephadex LH-20柱色谱等方法进行分离纯化,根据波谱学数据和理化性质进行结构鉴定。结果从西南山茶叶体积分数95%乙醇提取物的乙酸乙酯萃取物中分离并鉴定了11个化合物,分别为槲皮素(quercetin,1)、芦丁(rutin,2)、槲皮素-3-O-α-D-阿拉伯糖苷(quercetin-3-O-α-D-arabinofuranoside,3)、槲皮素-3-O-β-D-半乳糖苷(quercetin-3-O-β-D-galactopyranoside,4)、槲皮素-3-O-β-D-鼠李糖苷(quercetin-3-O-β-D-rhamno-side,5)、山柰酚(kaempferol,6)、山柰酚-3-O-(2″,6″-二反式-对香豆酰基)-β-D-葡萄糖苷(kaempfer-ol-3-O-[2″,6″-di-(E)-p-coumaroyl]-β-D-glucopyranoside,7)、羽扇豆醇(lupeol,8)、齐墩果酸(olean-olic acid,9)、原儿茶酸(3,4-dihydroxybenzoic acid,10)和没食子酸乙酯(ethyl gallate,11)。结论化合物1~11均首次从西南山茶中分离得到,其中化合物7为首次从山茶属植物中分离得到。