相转移催化合成对甲氧基肉桂酸-2-乙基己酯的研究

对甲氧基肉桂酸 2 乙基己酯是一种有效的ＵＶＢ防晒剂[1 ,2 ] ,一般采用Ｃｌａｉｓｅｎ Ｓｃｈｍｉｄｔ缩合反应制得[3] ,但由于催化剂ＫＯＨ处于水相 ,对反应物不能充分起到催化作用导致产率较低[4] 。我们利用乙二醇 (ＰＥＧ)为相转移催化剂合成立体专一的反式对甲氧基肉桂酸 2 乙基己酯 ,产率提高到 72 .5 %。合成路线如下 :1　实验部分1 .1　仪器与试剂ＢＩＯ ＲＡＰＦＴ45 0红外光谱仪 ,用液膜法测试 ;Ｂｒｕｒｅｒ ＡＭ 30 0超导核磁共振仪 (溶剂ＤＣ Ｃｌ3) ;ＭＡＴ/44Ｓ ,ＧＣ ＭＳ型色质联用谱仪 ;试剂均为分析纯 ,上海化学试剂…     

Resonance double light scattering method for the determination of proteins with morin-CTMAB

A new determination method of proteins with the limit of determination at nanogram levels is proposed by using a common spectrofluorimeter to detect intensity of resonance double line scattering (RDLS). Proteins including bovine serum albumin (BSA), human serum albumin (HSA) can combine with morin and cetyltrimethylammonium briomide (CTMAB) in the pH range 7.0-8.0 and produce enhanced RDLS signal at lambda(ex)/lambda(em) 305.0/610.0 nm. Optimization conditions for the morin-protein-CTMAB interaction were tested. In the studied system, BSA/CTMAB/morin = 1:2:3. The association constant of morin with BSA is 5.2 x 10(4). Under the optimum conditions, the linear range is 7.5 x 10(-8)-1.0 x 10(-5) g/ml for BSA, 2.5 x 10(-8)-5.0 x 10(-6) g/ml for HSA. The detection limits (S/N = 3) are 66.0 ng/ml for BSA and 23.0 ng/ml for HSA, respectively. Four synthetic samples were analyzed satisfactorily.     

羟基取代烷基苯磺酸盐界面扩张粘弹性质

研究了2-羟基-3,5-二癸基苯磺酸钠(C10C10OHphSO3Na)表面和正癸烷-水界面上的扩张粘弹性质, 考察了平衡时间对界面性质的影响. 研究结果表明, 羟基取代烷基苯磺酸钠具有十分特异的界面性质, 其扩张模量比一般表面活性剂大一个数量级, 达到平衡的时间较长, 形成的界面膜弹性较大. 界面张力弛豫测定结果表明, 平衡时界面上存在特征时间长达103 s的慢过程. 上述实验结果可能是由于羟基间形成氢键造成的.     

New bioactive triterpenoid from Oldenlandia cantonensis How

A new pentacyclic triterpenoid, urs-12-en-29α-oic acid-3β-ol (1), was obtained from the ethanol extract of Chinese herb Oldenlandia cantonensis How. The structure was elucidated by spectroscopy methods, including nuclear magnetic resonance (NMR) (1D and 2D), infrared spectroscopy (IR), and mass spectrometry (MS). 1 exhibited significant inhibitory activity against the human DNA topoisomerase I (hTopo I), the cancer cell lines BEL-7402 and MCG-803, with the IC₅₀ values 12.0, 6.5, and 8.0 μg/mL, respectively. The volatile oil, the fraction of petroleum ether: EtOAc = 20:1 (V/V) on Si gel chromatography, was also quantitatively analyzed by gas chromatography mass spectrometry (GC-MS). As a result, 60 compounds were identified. Among them, the long chain aliphatics, terpenes and steroids, as the representative structure type, were found with percentages of 36.16%, 6.42% and 9.28%, respectively. Translated from Chinese Journal of Applied Chemistry, 2006, 23(8): 871–874 [译自: 应用化学]     

Supercritical fluid extraction of flumetralin in tobacco

Summary This work evaluates the level of Flumetralin residues in real tobacco samples. Conventional extraction methods were compared with SFE methods in both static and dynamic modes using CO₂ and CO₂ with modifier. Additionally, in the dynamic SFE mode, different collection approaches, such as collection at room temperature without solvent, collection at room temperature in the presence of solvent (hexane) and collection in an ice bath, without solvent, were studied. SFE showed itself to be a promising extraction technique for pesticide residues in tobacco samples.     

LaxBa1—xCoO3系导电陶瓷导电性研究

对ＬａｘＢａ１－ｘＣｏＯ导电陶瓷的导电性及其导电机制进行了研究，在ｘ＝０．５ｍｏｌ处，导电陶瓷具有金属态导是性，在Ｌａ０．５Ｂａ０．５ＣｏＯ３陶瓷中，存在着氧缺位和导电电子，并且此种导电陶瓷具有较高的电子和氧离子混合导电特性。     

孔壁部分有序化的介孔二氧化硅材料的合成与表征

采用一种“改进的二次晶化”的方法处理介孔二氧化硅SBA-15. 用X射线衍射(XRD)、 透射电镜(TEM)、 电子衍射(ED)、 红外光谱(FTIR)以及固体核磁共振(NMR)等多种技术对样品进行了表征.　结果表明， 在所得样品的孔壁中, 原子的排列方式与普通介孔二氧化硅材料的孔壁不同， 显示一定程度的有序性. 同时, 高度有序的介孔结构得到很好的保持, 且样品的水热稳定性大幅度提高.     

紫杉醇的合成进展

紫杉醇是一种重要的抗癌药物,它具有复杂新颖的化学结构,为三环二萜类化合物.本文综述了紫杉醇的半合成和紫杉烷环的各种合成方法.     

黄烷类衍生物的合成及其生物活性研究

An efficient and feasible synthetic approach was developed for the synthesis of an array of new flavane derivafives from the substituted benzaldehyde with the reduction of chalcones and subsequent cyclization as the key steps. The purity and structure of the products were confirmed by the elemental analysis and a combination of its IR, ^1H and ^13C NMR, and mass spectra. These synthetic compounds were tested for xanthine oxidase （XO） inhibitions and antifungal actions against Candida albicans, Cryptococcus neoformans, Aspergillus sp. and Trichophyton rubrum. 7-Hydrazinocarbonylmethoxy-4＇-methoxyflavane （9） was found to be the most XO inhibitory with IC50=76.4 μmol/L, and the most potent antifungal compound was 4＇-hydrazinocarbonylmethoxyflavane （12） with minimal inhibition concentration MIC=8 μg/mL against Trichophyton rubrum.     

Study on Extraction Process of Root of Henry Wood Betony Polysaccharides and Their Antitumor Activity against S180

We optimized the hot water extraction of polysaccharides from the root of Henry wood betony (RHWPs) using a uniform test and explored their anti-tumor activities in vitro and in vivo. The optimal extraction conditions were as follows: 40 min extraction time, liquid/solid ratio 30 mL/g, 100 min soaking time, two extraction cycles, 100% ethanol concentration, and extraction temperature of 80 °C. The molecular weight distribution of RHWPs with MWs was 228,600 g/mol and 5001 g/mol. The IR spectrum further indicated that RHWPs are acidic polysaccharides containing pyranose and furan rings. The main monosaccharides found in RHWPs were mannose, ribose, l-rhamnose monohydrate, glucuronic acid, galacturonic acid, glucose, galactose, xylose, arabinose, and fucose. RHWPs inhibited the proliferation of S180 tumor cells and induced apoptosis in vitro. Oral administration of RHWPs to tumor-bearing mice significantly inhibited the growth of the S180 xenografts, accelerated apoptosis in tumor cells, and expanded the necrotic regions. Furthermore, RHWPs also markedly increased the levels of TNF-α, IFN-γ, and IL-2 in the sera of tumor-bearing mice, and activated immune cells such as lymphocytes, NK cells, and macrophages, thereby inducing tumor cell apoptosis. Taken together, RHWPs are a promising anti-tumor agent that ought to be explored further.