Constituents of Antrodia Cinnamomea

We describe identification of seven components from Antrodia cinnamomea. Their structures were determined on the basis of spectral analysis and comparison with authentic samples. These compounds include two steroids (1, 2) (β-sitosterol and eburicol), two new steroids (3, 4) [methyl-4α-methylergost-8,24(28)-dien-3,7,11-trion-26-oate and methyl-4α-methylergost-8,24(28)-dien-3,11-dion-26-oate], two lignans (5, 6) [(+)-sesamin and 4-hydroxysesamin], and one long chain methyl ester (7) (methyl oleate). Among them, compounds 3 and 4 are first isolated from nature.     

离子液体作添加剂对高效液相色谱分离植物激素的影响

探讨了以离子液体作为液相色谱流动相添加剂,对植物激素赤霉素GA3、生长素IAA和脱落酸ABA的分离的影响,以及离子液体的烷烃链长度,阴离子及离子液体的浓度对分离的影响。结果表明:咪唑阳离子和植物激素通过静电作用而保留;植物激素本身的pKa值影响其保留因子,pKa值增大,离子液体浓度对植物激素保留因子影响增大;另外随[BMIM]对应的阴离子电负性的减小,植物激素的保留因子明显地增大;同时植物激素的空间位阻也影响其分离。     

Capillary electrophoresis coupled to time of flight-mass spectrometry of therapeutic peptide hormones

We have established a method for separation and characterization of a series of peptide hormones of pharmaceutical interest and wide therapeutical use by capillary electrophoresis-electrospray-mass spectrometry (CE-ES-MS) using a sheath flow interface. Several parameters were systematically investigated, such as concentration of the electrolyte, organic solvent and sheath liquid composition, gas flow rates and capillary position. Moreover, limits of detection, linearity, repeatability and day-to-day reproducibility of the proposed method were studied in order to obtain the main quality parameters.     

Dexamethasone delivery to posterior segment of the eye

Due to anatomic barriers and lacrimal drainage it is difficult to obtain therapeutic drug concentrations in the posterior part of the eye after topical drug administrations. Lipophilic cyclodextrins, such as randomly methylated β-cyclodextrin (RMβCD), are known to act both as solubilizers of water-insoluble drugs in aqueous solutions and as penetration enhancers that reduce the barrier function of lipophilic membranes. The purpose of this study was to investigate the effects of RMβCD on dexamethasone delivery from aqueous eye drop solution into rabbit eyes. Dexamethasone (0.5 and 1.5% w/v) drops (50 μl) were administered to the left eye of rabbits (n = 6) and the drug levels measured in different eye tissues 2 h after administration. In aqueous humor dexamethasone levels were 1,190 ± 110 and 1,670 ± 630 ng/g (mean ± SD) after administration of the 0.5 and 1.5% dexamethasone eye drops, respectively. In the retina the levels were 33 ± 7 and 66 ± 49 ng/g, and in optic nerve 41 ± 12 and 130 ± 50 ng/g, respectively. In a previous study the dexamethasone concentration in aqueous humor after topical administration of 1.3% (w/v) dexamethasone eye drops in aqueous 2-hydroxypropyl-β-cyclodextrin (HPβCD) solution was determined to be 320 ± 230 ng/g and 66 ± 20 ng/g after administration of Maxidex^® eye drops. Both the hydrophilic HPβCD and the lipophilic RMβCD enhance topical dexamethasone delivery into the eye, but of the two, the lipophilic RMβCD results in higher dexamethasone concentrations.     

A new route for synthesizing cholesterol analogs with fluorocarbon side chains and their liquid-crystalline aliphatic esters

A new and efficient route has been developed to synthesize 17β-(1-methyl-3-perfluoroalkyl)propyl-3β-androsterol (1) in nine steps from hyodeoxycholic acid via selective addition of 1-perfluoroalkyl iodide to 24-norchola-5,22-dien-3β-ol. From (1), the first series of steroidal liquid crystalline aliphatic esters (smectic A) with fluorocarbon side chains has been prepared.     

梯度洗脱测定植物源调节剂中内源激素方法探讨

建立了梯度洗脱高效液相色谱法同时测定内源激素赤霉素(GA3)、吲哚乙酸(3-IAA)、脱落酸(ABA)、细胞分裂素(6-BA)和α-萘乙酸(α-NAA)等5种植物内源激素的方法,采用Hypersil ODS C18柱和紫外检测器,以甲醇、乙腈和0.6%的乙酸为流动相梯度洗脱,分别在各组分的保留时间段设置其最佳检测波长,在12 min内可将上述5种内源激素的各组分分离完全,峰形良好,该方法的回收率可达到90%～96%,线性相关系数(r)大于0.998,检出限在0.02～0.3 μg/g之间.还探讨了各组分的最佳检测条件和梯度洗脱存在的问题及解决方法.     

Simultaneous determination of acidic,basic and alcoholic substances relating to monoamine hormones and metabolites in biological material by mass fragmentography (GC/MF)

A method is described for the simultaneous quantitative determination of monoamines and related compounds from urine and brain tissue samples in the pg-range, using a GC/MF instrument LKB-2091 provided with a multiple ion detection (MID) system and capillary columns. The simultaneous detection of “fingerprints” with fourteen and more compounds during one single GC run was achieved after the intoduction of “time gates” for the detection of the different characteristic masses. Several modifications to the LKB equipment permitted exact reproducibility of retention times, which is essential for the use of “time gates”. The detection of “fingerprints” with these acidic, basic and alcoholic substances was achieved by the extraction of the dried biological samples with silylating agents.     

Kinetics of epidermal growth factor/receptor binding on cells measured by total internal reflection/fluorescence recovery after photobleaching

Total internal reflection fluorescence (TIRF) microscopy is used to measure the dissociation kinetic rate of fluorescein-labeled epidermal growth factor from its specific receptors on the surface of intact but mildly fixed A431 human epidermoid cells in culture. Prior applications of TIRF microscopy have been limited to nonreceptor binding or to model membrane systems. The evanescent field excites fluorescence selectively at the surface of the cell proximal to the coverslip. Prismless epiillumination TIR is employed to avoid space limitations and is achieved by passing the excitation laser beam through a high (1.4)-aperture objective so that the light is incident at the glass/water interface beyond the critical angle. Long-term focus is maintained by a special feedback system. Of the possible effects that can influence the time course of the postbleach fluorescence recoveries—the EGF/receptor dissociation ratek ₂, the bulk solution diffusion rate of EGF, and the cell surface motion of the receptors—we infer that the dissociation ratek ₂ dominates. Several fitting schemes are compared and indicate the presence of a multiplicity of values fork ₂, ranging from about 0.05 to 0.004 s^–1, with an average value of about 0.012 s^–1. These results compare well with values previously obtained by radiolabel/washing techniques. The significance of the results in terms of kinetic models and the advantages of the TIRF technique for these sorts of measurements are discussed.