卵叶娃儿藤中的抗癌活性生物碱

从卵叶娃儿藤(Tylophora ovata (Lindl.) Hook. ex Steud.)根中分离得到 4个菲骈吲哚里西丁类生物碱,分别为tylophoridicine A (1)、娃儿藤宁(2)、氧甲基娃儿藤定(3)和娃儿藤定(4).经波谱分析并结合化学方法鉴定,其结构分别为:(13aR)-6-羟基-3,7-二甲氧基菲骈吲哚里西丁、 (13aS ,14R)-14-羟基-3,6,7-三甲氧基-菲骈吲哚里西丁、(13aS, 14S)-14-羟基-3,6,7-三甲氧基-菲骈吲哚里西丁和(13 aS,14S)-6,14-二羟基-3,7-二甲氧基-菲骈吲哚里西丁.化合物1为新化合物,化合物2-4为首次从该植物得到的化合物.经药理筛选,化合物1、3和4显示很强的抗癌活性.     

红叶藤化学成分的研究

从红叶藤[Rourea microphylla(Hook.et Arn)Plan ch.]茎叶中分得11种化合物,经理化常数测定、光谱分析及化学方法鉴定为槲皮素-3-O-α-L-鼠李吡喃糖甙(Ⅰ)、金丝桃甙(Ⅱ),槲皮素(Ⅲ)、落新妇甙(Ⅳ)、β-谷甾醇(Ⅴ)、β-谷甾醇-β-D-葡萄吡喃糖甙(Ⅵ)、大黄素甲醚(ⅦI)、红灰青素(Ⅷ)、硬脂酸(Ⅸ)、软脂酸(Ⅹ)和正九烷(Ⅺ)。其中化合物Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅵ、Ⅶ、Ⅷ、Ⅸ、Ⅹ和Ⅺ为首次。从红叶藤属植物中分得。     

醉魂藤的化学成分研究

运用多种色谱技术从云南产醉魂藤Heterostemma alatum wight中分离得到10个化合物.通过理化鉴别和波谱数据确定了他们的化合物结构分别为β-谷甾醇(1)、正二十四烷酸(2)、芹菜素(3)、胡萝卜苷(4)、芹菜素-7-O-β-D-葡萄糖苷(5)、醉魂藤碱A(6)、醉魂藤碱B(7)、醉魂藤碱C(8)、醉魂藤碱D(9)和醉魂藤碱F(10).这些化合物均为首次从该植物中分离得到.     

卵叶娃儿藤中的抗癌活性生物碱

从卵叶娃儿藤 (Tylophoraovata (Lindl.)Hook .exSteud .)根中分离得到 4个菲骈吲哚里西丁类生物碱 ,分别为tylophoridicineA (1)、娃儿藤宁 (2 )、氧甲基娃儿藤定 (3)和娃儿藤定 (4 )。经波谱分析并结合化学方法鉴定 ,其结构分别为 :(13aR)_6_羟基_3,7_二甲氧基菲骈吲哚里西丁、(13aS ,14R)_14_羟基_3,6 ,7_三甲氧基_菲骈吲哚里西丁、(13aS ,14S)_14_羟基_3,6 ,7_三甲氧基_菲骈吲哚里西丁和 (13aS ,14S)_6 ,14_二羟基_3,7_二甲氧基_菲骈吲哚里西丁。化合物 1为新化合物 ,化合物 2 - 4为首次从该植物得到的化合物。经药理筛选 ,化合物 1、3和 4显示很强的抗癌活性。     

思茅藤的化学成分研究

从思茅藤(Epigynum auritum (schneid.)Tsiang et P.T.Li)的茎皮中分离到一个新的化合物,命名为思茅藤甙(Epigcoside)Ⅰ和已知化合物Ⅱ。通过光谱分析和化学反应证明,其结构为Ⅰ(+)—儿茶素-3-O-α-D-葡萄吡喃糖(1→6)-β-D葡萄吡喃糖甙((+)-catchin—3-O-α-D-glucopyranosyl-(1→6)-β—D-glucopyranoside;Ⅱβ-谷甾醇β-D-葡萄糖甙(β-sitosterol-β-D-glucoside)。     

贵州苗药黑骨藤化学成分的研究

利用色谱技术从黑骨藤(Periploca forrestii Schltr)中分离得到9个化合物,通过理化性质和光谱分析,分别鉴定为:α-香树脂醇(I),α-香树脂醇乙酸酯(Ⅱ),27-羟基-α-香树脂醇(Ⅲ),β-香树脂醇(IV),β-香树脂醇乙酸酯(V),熊果酸(Ⅵ),β-谷甾醇(Ⅷ),β-胡萝卜甙(Ⅷ),大黄素(Ⅸ).化合物Ⅰ,Ⅲ,Ⅳ,Ⅴ为首次从该植物中分离得到.     

雪兔子的成分研究

从雪兔子(Saussurea gossypiphora D.Don)中首次分得6种结晶物,经红外光谱、紫外光谱、质谱和核磁共振谱等方法鉴定为:伞形花内酯(umbelliterone)(Ⅰ)东莨菪素(scopole-tin)(Ⅱ),β-谷甾醇(β-sitosterol)(Ⅲ),芹菜素(apigenin)(Ⅳ),芹菜素7-葡萄糖甙(api-genin 7-O-β-D-glucoside)(Ⅴ),伞形花内酯甙(umbelliteione 7-O-β-D-glucoside)(Ⅵ)。     

叉子圆柏中的抗肿瘤化学成分

从叉子圆柏(Sabina vulgaris Ant.)的树皮中分得12种成分,根据其理化性质、化学反应及光谱分析,其中11种成分鉴定为反式璎珞柏酸(Ⅰ),顺式璎珞柏酸(Ⅱ),山达海松酸(Ⅲ),异柏油酸(Ⅳ)、柳杉酚(Ⅴ)、12-羟基-6,7-断松香烷8,11,13三烯6,7二醛(Ⅵ),β-足叶草素 A 早醚(Ⅶ),佛手内酯(Ⅷ),β-谷甾醇(Ⅹ),二十四烷酸(Ⅺ)和蜡酸(Ⅻ),另一种是新的3,4苯并香豆素类化合物,命名为圆柏内酯(sabilactone,Ⅸ),Ⅳ-Ⅹ为首次从该植物中分得。生物试验表明Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅵ和Ⅶ具有细胞毒作用。     

千金藤碱中的微量生物碱杂质

纯度达99.5%的千金藤碱经氧柱层析反复分离纯化,得到其中的微量杂质成分,通过波谱鉴定为（＋）-千金藤碱2＇-β-N-氧化物（1）.     

头序楤木化学成分研究

自头序楤木70%EtOH提取物分得6个化合物,应用光谱技术(IR,MS,(?)~HNMR,~(13)C NMR.DEPT,2DNMR)及化学方法.确定了他们的结构,分别为β-谷甾醇(Ⅰ),胡萝卜甙(Ⅱ),齐墩果酸(Ⅲ),竹节参皂甙 (?)(Ⅳ):竹节参皂甙Ⅳa(Chikusetsusapomin Ⅳa)(Ⅴ),常春藤皂甙元—28-O-β-吡喃葡萄糖醛酸(1→4)-β-D-吡喃葡萄糖甙(Ⅵ),以上化合物均为首次从该植物中分得,其中Ⅵ为一新化合物.     

The Chemical Constituents from Cynanchum Komarovii Al. Ilinski

Ten compounds were isolated from the roots and stems of Cynanchum komarovii Al. Iljinski. They were identified as 7-demethoxylophorine (Ⅰ), epi-alnusenol (Ⅱ), β-sitosterol (Ⅲ), triacontanolic acid (Ⅳ), sucrose (Ⅴ), desoxytylophorinin N-oxide (Ⅵ), apocynine (Ⅶ), paeonol (Ⅷ), β-sitosteryl-β-D-glucopyranoside (Ⅸ) and glucose (Ⅹ) by means of UV, IR, NMR, MS spectral analyses and through chemical methods. These compounds were first reported in this plant. One of them, Ⅵ is a new alkaloid. The bioassay results showed that the compounds Ⅰ, Ⅵ and reaction product Ⅺ exhibited cytotoxic effects to P-388 leukemia cell in vitro. Ⅺ is also a new compound.     

Determination of clozapine and its major metabolites in human plasma and red blood cells by high-performance liquid chromatography with ultraviolet absorbance detection

An isocratic high-performance liquid chromatographic (HPLC) method with UV absorbance detection is described for the quantification of clozapine (8-chloro-11-(4′-methyl)piperazino-5H-dibenzo[b,e]-1,4-diazepine) and its two major metabolites in plasma and red blood cells (RBCs). The method involves sample clean-up by liquid-liquid extraction with ethyl acetate. The organic phase was back-extracted with 0.1 M hydrochloric acid. Loxapine served as the internal standard. The analytes were separated by HPLC on a Kromasil Ultrabas C₁₈ analytical column (5 μm particle size; 250×4.6 mm I.D.) using acetonitrile-phosphate buffer pH 7.0 (48:52, v/v) as eluent and were measured by UV absorbance detection at 254 nm. The limits of quantification were 20 ng/ml for clozapine and N-desmethylclozapine and 30 ng/ml for clozapine N-oxide. Recovery from plasma or RBCs proved to be higher than 62%. Precision, expressed as % C.V., was in the range 0.6–15%. Accuracy ranged from 96 to 105%. The method's ability to quantify clozapine and two major metabolites simultaneously with precision, accuracy and sensitivity makes it useful in therapeutic drug monitoring.     

The Escherichia coli ynfEFGHI operon encodes polypeptides which are paralogues of dimethyl sulfoxide reductase (DmsABC)

The ynfEFGHI operon is a paralogue of the Escherichia coli dmsABC operon. ynfE and ynfF are paralogues of dmsA. ynfG and ynfH are paralogues of dmsB and dmsC, respectively. YnfI (dmsD) has no dms paralogue. YnfE/F and YnfG could be detected by immunoblotting with anti-DmsAB antibodies when expressed under the control of a tac or dms promoter. Cells harbouring ynfFGH on a multicopy plasmid supported anaerobic growth with dimethyl sulfoxide (DMSO) as respiratory oxidant in a dmsABC deletion, suggesting that YnfFGH forms a heterotimeric enzyme complex similar to DmsABC. Exchange of DmsC by YnfH (DmsAB-YnfH) resulted in membrane localization, anaerobic growth on DMSO, and binding of 2-n-heptyl 4-hydroxyquinoline-N-oxide, indicating that YnfH was a competent anchor. YnfG can also replace DmsB as the electron transfer subunit and assembled [Fe-S] clusters as judged by electron paramagnetic resonance spectroscopy. YnfE and/or YnfF could not form a functional complex with DmsBC and expression of YnfE prevented the accumulation of YnfFGH.     

苦参生物碱的研究

从苦参(Sophora flavescens Ait)根中分离得到9个生物碱,用波谱等方法确定为槐果碱(sophocarpine)、苦参碱(matrine)、异苦参碱(isomatrine)、槐醇(sophoranol)、N-甲基野靛碱(N-methylcytisine)、槐定(sophoridine)、氧化苦参碱(oxymatrine)、氧化槐果碱(oxysophocarpine)和氧化槐醇(sophoranol N-oxide)。其中氧化槐醇是首次从苦参根中得到的。     

Quantitation of sorafenib and its active metabolite sorafenib N-oxide in human plasma by liquid chromatography–tandem mass spectrometry

A simple and rapid method with high performance liquid chromatography/tandem mass spectrometry is described for the quantitation of the kinase inhibitor sorafenib and its active metabolite sorafenib N-oxide in human plasma. A protein precipitation extraction procedure was applied to 50 μL of plasma. Chromatographic separation of the two analytes, and the internal standard [²H₃¹³C]-sorafenib, was achieved on a C₁₈ analytical column and isocratic flow at 0.3 mL/min for 4 min. Mean within-run and between-run precision for all analytes were <6.9% and accuracy was <5.3%. Calibration curves were linear over the concentration range of 50–10,000 ng/mL for sorafenib and 10–2500 ng/mL for sorafenib N-oxide. This method allows a specific, sensitive, and reliable determination of the kinase inhibitor sorafenib and its active metabolite sorafenib N-oxide in human plasma in a single analytical run.     

Synthesis and characterization of pyridine N-oxide complexes of manganese, copper and zinc

A series of metal carboxylates containing pyridine N-oxide are prepared via one pot synthesis and solid phase synthesis. The structural variations from metal to metal are observed. In the case of reactions of manganese(II) acetate with pyridine N-oxide in the presence of aromatic carboxylic acids, polymeric complexes with bridging aromatic carboxylate as well as bridging pyridine N-oxide are observed. Whereas, the reaction of copper(II) acetate with pyridine N-oxide in the presence of an aromatic carboxylic acid led to mononuclear or binuclear paddle wheel carboxylate complexes with monodentate pyridine N-oxide. Co-crystal of two neutral complexes having composition [Cu₂(OBz)₄(MeOH)₂][Cu₂(OBz)₄(pyO)₂] (where OBz = benzoate, pyO = pyridine N-oxide) each neutral parts have paddle wheel structure. Solid phase reaction of zinc chloride with sodium benzoate prepared in situ and pyridine N-oxide leads to a tetra-nuclear zinc complex.     

Effects of silicon sources on its deposition, chlorophyll content, and disease and pest resistance in rice

Rice (Oryza sativa L.) was grown in pots with pyridine N-oxide (PNO), 4-morpholino pyridine N-oxide (MNO), and sodium meta silicate as the sources for silicon. Aliquots of these were added in fortnightly intervals to seedlings through anthesis stage. The plants were monitored for plant growth characteristics, chlorophyll content (SPAD values), photosystem 2 activity (variable to maximum fluorescence ratio of dark adapted leaves), and for blast and yellow stem borer resistance. Deposition of silica in the leaves was monitored by scanning electron microscopy and silicon mapping. PNO or MNO application resulted in significant silicon accumulation in leaf bundle sheath cells. Application of PNO and MNO imparted disease and pest resistance by increasing silicon uptake of rice plants.     

Aporphine Alkaloids from Ocotea puberula with Anti-Trypanosoma Cruzi Potential – Activity of Dicentrine-β-N-Oxide in the Plasma Membrane Electric Potentials

One new aporphine, dicentrine-β-N-oxide ( 1 ), together with five related known alkaloids dehydrodicentrine ( 2 ), predicentrine ( 3 ), N-methyllaurotetanine ( 4 ), cassythicine ( 5 ), and dicentrine ( 6 ) were isolated from the leaves of Ocotea puberula (Lauraceae). Antiprotozoal activity of the isolated compounds was evaluated in vitro against trypomastigote forms of Trypanosoma cruzi. Among the tested compounds, alkaloid 1 exhibited higher potential with EC₅₀ value of 18.2 μM and reduced toxicity against NCTC cells (CC₅₀>200 μM – SI>11.0), similar to positive control benznidazole (EC₅₀ of 17.7 μM and SI=10.7). Considering the promising results of dicentrine-β-N-oxide ( 1 ) against trypomastigotes, the mechanism of parasite death caused by this alkaloid was investigated. As observed, this compound reached the plasma membrane electric potential directly after 2 h of incubation and triggered mitochondrial depolarization, which probably leads to trypomastigote death. Therefore, dicentrine-β-N-oxide ( 1 ), reported for the first time in this work, can contribute to future works for the development of new trypanocidal agents.     

Simultaneous measurement of nicotinamide and its catabolites,nicotinamide N-oxide,N1-methyl-2-pyridone-5-carboxamide,and N1-methyl-4-pyridone-3-carboxamide,in mice urine

Nicotinamide N-oxide is a major nicotinamide catabolite in mice but not in humans and rats. A high-performance liquid chromatographic method for the simultaneous measurement of nicotinamide, nicotinamide N-oxide, N¹-methyl-2-pyridone-5-carboxamide, and N¹-methyl-4-pyridone-3-carboxamide in mice urine was developed by modifying the mobile phase of a reported method for measurement of nicotinamide N-oxide.     

Field-amplified sample stacking in capillary electrophoresis for the determination of clozapine, clozapine N-oxide, and desmethylclozapine in schizophrenics' plasma

A method of field-amplified sample stacking in capillary electrophoresis is described for the simultaneous determination of clozapine (CZP) and its metabolites, clozapine N-oxide (CNO), and desmethylclozapine (DMC), in human plasma. Plasma (0.2 mL) was extracted with organic solvents (ethyl acetate/n-hexane/isopropyl alcohol, 8/1/1 by volume) and centrifuged. An aliquot of supernatant was evaporated and suitably reconstituted with water for CE analysis. An untreated fused-silica capillary was used (31.2 cm; effective length, 20 cm; 50 microm i.d.) for the analysis. The background buffer was phosphate buffer (400 mM, pH 3.0) containing 50% ethylene glycol. The separation voltage was 25 kV with a detection wavelength of 214 nm. In the method validation, the calibration curves were linear (r > or = 0.98) over a range of 50-800 ng/mL for CZP, 30-180 ng/mL for CNO, and 25-600 ng/mL for DMC. The relative standard deviation (R.S.D.) and relative error (R.E.) were all less than 11% for the intra- and inter-day assays. The limits of detection (S/N = 3, electric-driven injection, 99.9s) of CZP, DMC, and CNO were 5, 5, and 10 ng/mL, respectively. After continuing treatment with the CZP tablets, a blood sample from one male schizophrenic patient (41-year-old, 62 kg) who had been receiving ongoing treatment with the CZP tablets was prepared and analyzed. The levels of CZP, DMC, and CNO were determined and the feasibility of the method's application in clinical treatment was proven.