岗松枝叶正丁醇萃取部位的化学成分

从岗松（Baeckea frutescens L.）枝叶正丁醇萃取部位分离鉴定了12个化合物，分别为：槲皮素（1），杨梅素（2），槲皮素3-O-α-L-吡喃鼠李糖苷（3），杨梅素3-O-α-L-吡喃鼠李糖苷（4），槲皮素3-O-α-L-呋喃阿拉伯糖苷（5），槲皮素3-O-β-D-吡喃木糖苷（6），槲皮素3-O-α-L-吡喃阿拉伯糖（7），槲皮素4′-O-β-D-吡喃葡萄糖苷（8），山柰酚 3-O-α-L-呋喃阿拉伯糖苷（9），山柰酚3-O-α-L-吡喃鼠李糖苷（10），myricetin 3-O-（2′′-O-galloyl）-α-L-rhamnopyranoside（11），myricetin 3-O-（3′′-O-galloyl）-α-L-rhamnopyranoside（12）。其中化合物5~12为首次从该植物枝叶中分离得到。     

甘青铁线莲的黄酮苷类成分研究

目的研究甘青铁线莲Clematis tangutica全草的黄酮类成分。方法甘青铁线莲全草经乙醇提取,依次用石油醚、水饱和正丁醇萃取,对正丁醇部位采用硅胶柱色谱、Sephadex LH-20凝胶色谱及半制备型HPLC等方法进行分离,根据理化性质和波谱分析鉴定化合物的结构。结果分离并鉴定了6个黄酮苷类化合物,分别为芹菜素-7-O-β-D-(-6’’-p-香豆酰基)-吡喃葡萄糖苷(1)、槲皮素-3-O-β-D-吡喃半乳糖-7-O-β-D-吡喃葡萄糖苷(2)、异荭草素(3)、槲皮素-3-O-β-D-吡喃半乳糖苷(4)、木犀草素-7-O-β-D-吡喃葡萄糖苷(5)和芹黄春(6)。结论化合物1为首次从铁线莲属中获得,所有化合物均为首次从该种植物中获得。     

红松松针中黄酮类成分的分离与鉴定

目的研究红松松针中的黄酮类成分,为松属植物的化学分类学研究提供依据。方法采用反复硅胶、聚酰胺、ODS、Sephadex LH-20柱色谱等方法进行分离纯化,根据理化性质和1H-NMR、13C-NMR等技术对分离得到的化合物进行结构鉴定。结果从红松松针中分离得到7个化合物,分别鉴定为蛇葡萄素4′-O-β-D-吡喃葡萄糖苷[ampelopsin 4′-O-β-D-glucopyranoside,1]、槲皮素3-O-α-L-呋喃阿拉伯糖苷[quercetin3-O-α-L-arabinofuranoside,2]、山柰酚3-O-α-L-呋喃阿拉伯糖苷[kaempferol3-O-α-L-arabinofuranoside,3]、山柰酚3-O-β-D-吡喃葡萄糖苷[kaempferol3-O-β-D-glu-copyranoside,4]、5,7,8,4′-四羟基-3-甲氧基-6-甲基黄酮8-O-β-D-吡喃葡萄糖苷[5,7,8,4′-tetra-hydroxy-3-methoxy-6-methylfavone8-O-β-D-glucopyranoside,5]、山柰酚3-O-(5″-O-反式-阿魏酰基)-α-L-呋喃阿拉伯糖苷[kaempferol3-O-(5″-O-E-feruloyl)-α-L-arabinofuranoside,6]、山柰酚3-O-(5″-O-反式-对-香豆酰基)-α-L-呋喃阿拉伯糖苷[kaempferol3-O-(5″-O-E-p-coumaroyl)-α-L-arabi-nofuranoside,7]。结论化合物1-3为首次从松属植物中分离得到,4-7为首次从该种植物中分离得到。     

野雉尾金粉蕨中一个新的大环黄酮

采用大孔树脂、硅胶、反相硅胶、葡聚糖凝胶及高效液相等色谱法,从野雉尾金粉蕨中分离纯化得到7个化合物。通过核磁共振谱、质谱等波谱学方法分别鉴定为金粉蕨酮A(1)、槲皮素(2)、槲皮素-3-O-α-L-吡喃鼠李糖苷(3)、山柰酚-7-O-β-D-葡萄糖苷(4)、山柰酚-3-O-α-L-吡喃鼠李糖苷(5)、(-)-prunin(6)和1,3,6,7-四羟基酮(7),其中化合物1为结构新颖的大环黄酮类化合物,其余化合物均为首次从该植物中分离得到。采用MTS法测试化合物对5种肿瘤细胞株的细胞毒活性,结果显示化合物7对肺癌A549、肝癌SMMC-7721和结肠癌SW480细胞具有弱的细胞增殖抑制活性。     

中国沙棘果实的化学成分及其体外抗氧化活性研究

目的 研究中国沙棘果实的化学成分,并测定部分化学成分体外活性.方法 采用95%乙醇渗滤提得总浸膏,经溶剂萃取及柱层析分离,采用化学及光谱方法进行结构鉴定,并对小鼠视网膜色素上皮细胞(RPE)建立H2O2损伤模型,使用3种单体与细胞共孵育,进行MTT检测分析.结果 分得3个新化合物,分别鉴定为异鼠李素-3-O-β-D-(6-O-反式芥子酰基)槐二糖-7-O-α-L-鼠李糖苷(Ⅰ)、山柰素-3-O-β-D-(6-O-反式芥子酰基)槐二糖-7-O-α-L-鼠李糖苷(Ⅱ)和槲皮素-3-O-β-D-(6-O-反式芥子酰基)槐二糖-7-O-α-L-鼠李糖苷(Ⅲ).化合物Ⅲ对RPE有抗氧化活性,化合物Ⅰ则无,槲皮素活性最强.结论 研究结果可为中国沙棘的临床应用提供理论依据.     

白枪杆的化学成分研究（I）

目的：研究木犀科辛琴属植物白枪杆的化学成分。方法：采用80％乙醇提取白枪杆树皮,以硅胶、凝胶等色谱手段分离化合物,经红外光谱、核磁共振光谱和质谱鉴定化合物结构。结果：共分离得到10个化合物,分别鉴定为咖啡酸甲酯（1）、1-O-咖啡酰基-α-D-葡萄吡喃糖（2）、1-O-咖啡酰基-βD-葡萄吡喃糖（3）、存额阿塔斯德A（4）、7,11．二甲酯油苷（5）、（8Z）．橄榄苦苷（6）、肌醇（7）、邻苯二酚（8）、α-乙基-D-呋喃葡糖苷（9）和β-甲基-L-吡喃鼠李糖苷（10）。结论：化合物1～10均为首次从白枪杆中分离得到。本研究结果可为了解该植物的特性提供-定依据。     

番石榴叶的化学成分

目的研究番石榴叶的化学成分。方法运用多种色谱技术方法对番石榴叶的化学成分进行了系统的研究,并根据波谱数据和理化性质确定了其结构。结果分离鉴定了7个化合物,分别为槲皮素-3-O-α-L-吡喃阿拉伯糖苷(quercetin-3-O-α-L-arabinopyranoside,1)、槲皮素-3-O-α-L-呋喃阿拉伯糖苷(quercetin-3-O-α-L-arabinofuranoside,2)、槲皮素-3-O-β-D-吡喃半乳糖(quercetin-3-O-β-Dgalactopyanoside,3)、2α,3β-二羟基乌索烷(2α,3β-di-hydroxy-ursane,4)、madecassic acid(5)、(7R,8S)二氢脱氢二松柏醇-9-O-β-D-吡喃葡萄糖苷((7S,8R)-5-methoxydehydrodiconiferyl alcohol-9-β-D-glucopyranoside,6)、quadranoside III(7)。结论化合物4-7为首次从番石榴属中分离得到。     

升麻中环菠萝蜜烷三萜化学成分及其抗肿瘤活性的研究

目的从常用中药升麻中分离鉴定具有抗肿瘤活性的环菠萝蜜烷三萜成分。方法应用正、反相硅胶(RP-18)柱层析,葡聚糖凝胶(Sephadex LH-20)柱层析,结合重结晶方法进行分离纯化;运用1H-NMR、13C-NMR、IR和MS等现代波谱技术对化合物的结构进行鉴定;采用MTT法测试化学成分对4种人肿瘤细胞增殖的抑制作用。结果从升麻乙醇提取物中分离了6个化合物,分别鉴定为:25-O-乙酰基-7,8-去氢升麻醇-3-O-β-D-吡喃木糖苷(1)、25-O-乙酰基-3-O-β-D-吡喃木糖苷(2)、7,8-去氢升麻醇-3-O-β-D-吡喃木糖苷(3)、升麻醇-3-O-β-D-吡喃木糖苷(4)、24-acetylisodahurinol-3-O-β-D-xylopranoside(5)、升麻酮醇-3-O-β-L-阿拉伯糖苷(6)。化合物1~6对4种人肿瘤细胞株Hep G2(肝癌)、MCF-7(乳腺癌)、Hela(子宫颈癌)、A549(肺癌)的增殖均有一定的抑制作用,其中化合物1对MCF-7和Hep G2作用较为明显,IC50值分别为17.7和22.0μmol·L-1。结论化合物5为首次从升麻中分离得到,化合物1具有潜在的抗肿瘤活性。     

猴耳环叶化学成分的分离与鉴定

目的研究猴耳环的化学成分。方法利用各种色谱法进行分离,根据理化性质和波谱分析鉴定化合物结构。结果从猴耳环的水提取物中分离得到8个已知成分,分别鉴定为lauroside D(1)、杨梅素-3-O-α-L-吡喃鼠李糖苷(myricitrin,2)、槲皮素-3-O-α-L-吡喃鼠李糖苷(quercitrin,3)、苯甲基-O-β-D-吡喃葡萄糖苷(benzyl-O-β-D-glucopyranoside,4)、没食子酸甲酯(methyl gallate,5)、没食子酸乙酯(ethyl gallate,6)、水杨酸甲酯-2-O-β-D-葡萄糖苷(methyl 2-O-β-D-glucopyranosylbenzoate,7)、canthoside A(8)。结论化合物1、4、7、8为首次从该属植物中分离得到。     

远志地上部分10个黄酮类成分的分离及抗氧化活性研究(英文)

研究远志地上部分的化学成分并测试其抗氧化活性。运用硅胶、Sephadex LH-20、ODS及半制备液相,从远志地上部分中分离得到10个黄酮类化合物。用DPPH自由基清除试验测定了其抗氧化活性。分离所得化合物经光谱数据分析鉴定其结构分别为:异鼠李素-3-O-β-D-吡喃葡萄糖苷(1),异鼠李素-3-O-β-D-吡喃半乳糖苷(2),槲皮素-3-O-β-D-吡喃葡萄糖(1→2)-β-D-吡喃半乳糖苷(3),槲皮素-3-O-β-D-吡喃葡萄糖(1→2)-β-D-吡喃葡萄糖苷(4),蒙花苷(5),槲皮素-3-O-β-D-吡喃葡萄糖苷(6),5,7-二羟基-3-甲氧基黄酮-7-O-β-D-葡萄糖醛酸(7),异鼠李素(8),山奈酚(9)和槲皮素(10)。所有化合物均为首次从该植物中分离得到,化合物1–5和7均为首次从该属植物中分离得到。活性测试结果表明,化合物3、4、6、8、9和10表现出一定的抗氧化活性。     

Triterpenoids from<Emphasis Type="Italic">Schisandra henryi</Emphasis> with cytotoxic effect on leukemia and hela cells<Emphasis Type="Italic">in vitro</Emphasis>

Four known lanostane triterpenoids, schiprolactone A (1), schisanlactone B (2), nigranoic acid (3) and schisandronic acid (4) were isolated from the stems of Schisandra henryi for the first time. Their structures were characterized by IR, MS and NMR techniques. Compounds 1, 2 and 4 showed moderate cytotoxic activity against Leukemia cells in vitro. Cytotoxic activity of compounds 1-4 showed IC50 of 0.0097, 0.01, 0.097 and 0.0099 micromol/mL respectively toward Leukemia cells and IC50 of 0.097, 0.1, 0.097 and 0.099 micromol/mL toward Hela cells respectively. It is the first report that these compounds possess cytotoxic activity on Leukemia and Hela cells.     

Isolated perfused lung extraction and HPLC-ESI-MS(n) analysis for predicting bioactive components of Saposhnikoviae Radix

A novel strategy for predicting bioactive components in traditional Chinese material herb was proposed, using isolated perfused rat lung (IPL) extraction and high performance liquid chromatography\tandem mass spectrometry (HPLC-MS(n)) analysis. The hypothesis is that when the IPL is perfused with the extract of Saposhnikoviae Radix (ESR), the potential bioactive components in the ESR should selectively combine with the receptor or channel of lung, by changing the pH of perfused liquid, the combining components would be eluated and then detected by HPLC-ESI-MS(n). Five compounds were detected in the desorption eluate of IPL; among these compounds, two potential bioactive compounds, prim-O-glucosylcimifugin (2) and 4'-O-β-D-glucosyl-5-O-methylvisamminol (4) were identified by comparing with the chromatography of the standard sample, and three other compounds, i.e. cimifugin (1), 5-O-methylvisamminol (3) and sec-O-glucosylhamaudol (5) were determined by analysis of the structure clearage characterization of mass spectrometry. The application of IPL extraction coupled with HPLC-ESI-MS(n) for predicting potential bioactive components of TCMs is rapid, convenient, operational, economic and reliable.     

10-羟基喜树碱衍生物的合成及体外抑制肿瘤活性

目的寻找高效低毒的喜树碱类抗肿瘤新药。方法合成7个喜树碱衍生物（3~9），经¹HNMR，IR，MS分析确证了所合成化合物的结构，经MTT法筛选了对宫颈癌Hela、肝癌BEL-7402、胃癌7901和大肠癌CCL-187瘤株的体外抑制肿瘤活性。结果7个化合物分别对前三种瘤株有效，其中化合物4对前三种瘤株均有较好的体外抑制肿瘤细胞活性，尤其对宫颈癌Hela细胞的抑制活性大于10-羟基喜树碱。结论该类化合物的抗癌活性值得进一步研究。     

东北红豆杉及其伤愈组织粗提物中紫杉醇的HPLC-ESI-MS/MS分析研究

目的研究紫杉醇的二级质谱裂解规律，对东北红豆杉及其伤愈组织粗提物中的紫杉醇进行HPLC-ESI-MS/MS分离定性，为天然产物中该化合物的分离分析提供一种快速可靠的方法。方法对HPLC-ESI-MS/MS条件进行优化，研究紫杉醇电喷雾质谱的一级电离规律和二级质谱裂解规律，并结合液相色谱的保留时间判断东北红豆杉及其伤愈组织粗提物中紫杉醇色谱峰的归属。结果详细阐明了紫杉醇的二级质谱裂解规律，并利用HPLC-ESI-MS/MS法准确快速地分离定性了两种粗提物中紫杉醇。结论本方法灵敏度高，快速，选择性高，专属性好，能够作为天然产物及其产品中紫杉醇分离定性的一种快速可靠的技术手段。     

Aurora-B激酶抑制药的筛选和抗肿瘤活性研究

目的:以酵母细胞为模式菌高通量筛选具有抗肿瘤活性的Aurora-B激酶抑制药.方法:以野生型酵母菌Y300和ipl1-321温度敏感型突变株为模式菌,筛选Aurora-B激酶抑制药;体外酶学实验验证候选化合物对Aurora-B激酶的抑制作用;MTT方法检测阳性化合物对肿瘤细胞的杀伤活性;流式细胞术检测阳性化合物对肿瘤细胞的周期阻滞.结果:经筛选得到12个化合物和5个微生物发酵液;其中浓度在10μg·ml-1时对重组纯化的人Aurora-B激酶活性抑制率高于50%的有7个,其中3个活性较好的化合物IC50分别为10.253,1.826和2.054μmol·L-1;其中3个化合物对Hela细胞的IC50分别为4.255,15.326和1.032μmol·L-1,对HepG2细胞的IC50分别为5.387,17.465和1.725 μmol·L-1,对HCT116细胞的IC50分别为5.380,8.528和2.029 μmol·L-1.11号化合物能够诱导HCT116细胞G2/M期阻滞.结论:以Y300和ipl1-321酵母细胞为高通量筛选模型筛选到多个新的具有抗肿瘤活性的Aurora-B激酶抑制药.     

咪唑啉-2-酮衍生物的合成及其抗肿瘤活性

目的设计、合成五元环为咪唑啉-2-酮的CA-4的构象限制类似物，以期得到在体内外具有更好活性的化合物。方法取代苯胺与固体光气反应得取代苯异氰酸酯，不经后处理直接与相应的α-氨基苯乙酮盐酸盐在甲苯存在下回流反应得到3,4-二取代苯基-咪唑啉-2-酮-1-甲酰苯胺和3,4-二取代苯基-咪唑啉-2-酮。经MTT法筛选其对PC-3，A549，HO-8910，Hela，HL60，K562和HL60R瘤株的抗肿瘤活性，并对化合物4y进行了初步的作用机制研究。结果按上法制得36个未见文献报道的化合物，其结构经¹H NMR，MS和元素分析确证。结论体外活性测试表明，化合物4y对人白血病具有选择性的抑制作用，其作用机制主要为诱导凋亡。     

The antinociceptive effects of magnesium sulfate and MK-801 in visceral inflammatory pain model: The role of NO/cGMP/K+ATP pathway

Abstract

Context: Magnesium and MK-801 (dizocilpine), antagonists of N-methyl-d-aspartate receptors, are involved in the processing of pain.

Objective: This study determines whether magnesium sulfate (MS) and MK-801 affects visceral inflammatory pain and determines a possible mechanism of action.

Materials and methods: Analgesic activity was assessed using the acetic acid-induced writhing test in rats. MS (1–45?mg/kg) or MK-801 (0.005–0.03?mg/kg) was administrated subcutaneously (s.c.). To assess possible mechanisms of action, we examined the effects of l-NAME (10?mg/kg, intraperitoneal), methylene blue (0.5?mg/kg, s.c.), and glibenclamide (3?mg/kg, s.c.) on the effect of MS or MK-801.

Results: MS and MK-801 showed biphasic and linear dose–response pattern, respectively. MS reduces the number of writhing on the dose of 1, 5, and 15?mg/kg by 60, 50, and 78%, respectively, while it has no effects on the doses of 30 and 45?mg/kg. MK-801 (0.005–0.03?mg/kg) showed decrease in the number of writhing by 33–79%. The mean effective doses of MS and MK-801 were 6.6 (first phase) and 0.009?mg/kg, respectively. Both drugs did not impair the rotarod performance. l-NAME, methylene blue, and glybenclamide reduced the effect of MK-801 by 100, 43, and 64%, respectively, but not the effect of MS.

Conclusions: The results suggest that MS and MK-801 may be useful analgesics in the management of visceral inflammatory pain, at doses that do not induce motor impairment. The modulation of NO/cGMP/K+ATP pathway plays an important role in the antinociceptive mechanism of MK-801, but does not contribute to the antinociceptive effect of MS.     

HPLC-DAD and HPLC-ESI-MS/MS methods for metabolite profiling of propolis extracts

In this study, the composition of polyphenols (phenolic acids and flavonoids) in propolis extracts was investigated by HPLC-DAD and HPLC-ESI-MS/MS by comparing the performance of ion trap and triple quadrupole mass analyzers. The analyses were carried out on an Ascentis C(18) column (250mm×4.6mm I.D., 5μm), with a mobile phase composed by 0.1% formic acid in water and acetonitrile. Overall, the UV spectra, the MS and MS/MS data allowed the identification of 40 compounds. In the case of flavonoids, the triple quadrupole mass analyzer provided more collision energy if compared with the ion trap, originating product ions at best sensitivity. The HPLC method was validated in agreement with ICH guidelines: the correlation coefficients were >0.998; the limit of detection was in the range 1.6-4.6μg/ml; the recovery range was 96-105%; the intra- and inter-day %RSD values for retention times and peak areas were found to be <0.3 and 1.9%, respectively. The developed technique was applied to the analysis of hydroalcoholic extracts of propolis available on the Italian market. Although the chromatographic profile of the analyzed samples was similar, the quantitative analysis indicated that there is a great variability in the amount of the active compounds: the content of total phenolic acids ranged from 0.17 to 16.67mg/ml and the level of total flavonoids from 2.48 to 41.10mg/ml. The proposed method can be considered suitable for the phytochemical analysis of propolis extracts used in phytotherapy.     

HPLC-ESI-MS法同时检测抗风湿中成药制剂中非法添加肾上腺糖皮质激素类化学药品泼尼松等6种成分研究

目的:建立HPLC-ESI-MS法测定中成药制剂抗风湿药中有可能非法添加地塞米松、醋酸地塞米松、醋酸氢化泼尼松、醋酸氟氢松、氢化可的松、醋酸泼尼松等6种常用肾上腺糖皮质激素类化学药成分。方法:采用液质联用技术测定。色谱条件:Thermo ODS HYPERSIL(2.1μm×150mm,5μm)色谱柱,以乙腈-水梯度洗脱,检测波长240nm,流速0.2mL·min-1,进样量20μL;质谱条件:离子源为电喷雾离子化源(ESI源),源喷雾电压4500v,加热毛细管温度270℃,鞘气(N2)10,辅气(N2)20,正离子方式检测,扫描方式为一级全扫描、二级全扫描质谱,扫描范围150～550,扫描时间为0.129s。结果:根据检测到的化合物的色谱保留时间及一级、二级质谱信息,并与对照品比较,可作为分析检测中药制剂中非法添加上述6种肾上腺糖皮质激素类化学药的有效手段。结论:该检测方法选择性强,灵敏度高,定性准确。     

Synthesis and cytotoxicity of novel chrysin derivatives

A series of chrysin derivatives 8a–8v were prepared and tested in vitro against HCT-116 (human colon cancer cell line), Hela (human cervical carcinoma cell line), DU-145 (human prostate cell line), K562 (human leukemia cell line), and SGC-7901 (human gastric cancer cell line). The chemical structures of these compounds were confirmed by means of MS, IR, ¹H NMR, ¹³C NMR, and elemental analysis. Among these derivatives, 7-(2-(piperazin-1-yl)ethoxy)-5-hydroxy-2-phenyl-4H-chromen-4-one, 8n, had the strongest activity against HCT-116, Hela, DU-145, K562, and SGC-7901 cells. .