应用质谱扫描测定胸腺肽相对分子质量

目的 精确测定胸腺肽相对分子质量分布。方法 采用质谱扫描法。结果 3批胸腺肽相对分子质量均在2000～4000,无10 000以上的大分子蛋白。结论 本方法灵敏度高,可直观地测定胸腺肽相对分子质量分布状况,为控制胸腺肽质量提供了新的检测方法。     

4-(α-吡啶甲酰基)-PMP的合成与谱学特性研究

合成了新吡唑啉酮类试剂1-苯基-3-甲基-4-(α-吡啶甲酰基)-吡唑啉-5-酮(简称4-(α-吡啶甲酰基)-PMP,下同)。在表征分子结构的同时,对其红外、紫外吸收光谱,核磁共振氢谱、碳谱,质谱等谱学特性和质谱裂解规律进行了分析与研究。     

THE ROLE OF INTERFACIAL PHENOMENA IN A LIQUID-LIQUID REACTION SYSTEM: EXTRACTION OF PROPANOIC ACID BY TRIOCTYLAMINE

The kinetics of extraction of propanoic acid from water to isobulanol by reaction with trioctylamine have been investigated. Mass transfer was modelled by extending the approach used in absorption with chemical reaction, as it is usually done for liquid-liquid reactions. The presence of the amine, however, gave rise to phenomena that cause this method to fail, producing inconsistent results. In order to explain these data, the presence of relevant interfacial phenomena must be supposed.     

Method for characterization of triacylglycerols and fat-soluble vitamins in edible oils and fats by supercritical fluid chromatography

This study demonstrates the usefulness of capillary supercritical fluid chromatography (SFC) for the characterization of triacylglycerols of edible oils and fats. Triacylglycerols were separated according to the acyl carbon number and the degree of unsaturation on a 25% cyanopropyl/25% phenyl/50% methylpolysiloxane stationary phase. Valuable information concerning the triacylglycerol composition of berry oils was obtained, despite the overlapping of certain triacylglycerol peaks. Simultaneous analysis of fat-soluble vitamins and triacylglycerols is not practical by capillary SFC with flame-ionization detection because of the low concentration of naturally-occurring fat-soluble vitamins in edible oils. Therefore, higher loading of the sample, which led to overloading of triacylglycerols, was required to get reasonable peaks for fat-soluble vitamins. The method was applied to the characterization of triacylglycerols and tocopherols in sea buckthorn pulp and seed oil, and cloudberry seed oil without any sample purification prior to SFC. In addition, the stationary phase proved useful for separating the more complex mixtures of triacylglycerols found in milk fat and in fish oil.     

Simultaneous measurement of gas hold-up and mass transfer coefficient by tracer dynamic technique in “Emulsair” reactor with an emulsion-venturi distributor

Hydrodynamics and gas-liquid mass transfer have been investigated in an “Emulsair” reactor with cocurrent downflow of gas and liquid. This consists of a cylindrical tank with conical bottom topped by an emulsion-venturi as the gas-liquid distributor in which the gas is self-aspired by action of the kinetic energy of the liquid recirculation. An original tracer dynamic technique using the CO₂-N₂/water system that enables the simultaneous measurement of overall gas hold-up and overall volumetric mass transfer coefficient has been developed and validated using conventional techniques, such as volume expansion for gas hold-up and dynamic oxygenation for mass transfer. It has been shown that gas hold-up and K_La_L can be deduced from the moments of experimental response curves using a CO₂ pulse in the gas feed. Experimental results have proved that hydrodynamics and mass transfer in the Emulsair reactor are strongly influenced by the flow regime in the divergent. Two different regimes have been observed depending on the liquid recirculation flow rate: annular and homogeneous bubbling flows. In both regimes, self-aspired gas flow rate, gas hold-up and K_La_L have been reported to increase with the liquid flow rate. The operation effectiveness, estimated from the gas-to-liquid flow rate ratio, has been shown to pass through a maximum around 0.59 as a function of liquid recirculation. A comparison with the literature proved that this maximum is higher than those observed for other kinds of gas-liquid reactors equipped with a venturi. Correlations for mass transfer estimation have been derived and are in agreement with the literature.     

Matrix‐assisted laser desorption/ionization mass spectrometry of synthetic polymers. VI. Analysis of phenol–urea–formaldehyde cocondensates

Phenolic resoles can be regarded as copolymers of phenol and formaldehyde that are distributed in the chain length and the number of methylol groups per molecule. While other spectroscopic methods like FTIR and NMR only give average structures, MALDI–TOF mass spectrometry is able to resolve the oligomer distribution of phenolic resoles. Using 2,5‐dihydroxybenzoic acid or 2,4,6‐trihydroxyacetophenone as matrices, MALDI–TOF spectra are obtained where each oligomer peak can be assigned to a particular chemical structure. Thus, the degree of polymerization and the number of reactive methylol groups can be determined. For urea‐modified resoles, in addition to phenol–formaldehyde and urea–formaldehyde structures, for the first time, phenol–urea–formaldehyde cocondensate structures can be identified directly. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 2540–2548, 2003     

2-(5-溴-2-噻唑偶氮)-5-二乙氨基苯酚的合成与结构分析

用2-氨基噻唑为原料经溴化和重氮化,与N,N-二乙基间氨基苯酚偶联,合成了新有机分析试剂2-(5-溴-2-噻唑偶氮)-5-二乙氨基苯酚〔2-(5-Bromo-2-thiazolylazo)-5-diethylaminophenol,简称5-Br-TADAP〕.用薄层色谱法、元素分析法、质谱法、红外吸收光谱法、核磁共振谱法和可见吸收光谱法等分析手段对产品进行了分析和结构鉴定.该试剂至今未见文献报导.     

Experimental and theoretical study of membrane-aerated biofilm reactor behavior under different modes of oxygen supply for the treatment of synthetic wastewater

This study compares, experimentally and theoretically, five different modes of supplying oxygen to a membrane-aerated biofilm reactor (MABR), and search for the more efficient ways of treating wastewaters. A single-tube MABR was used to measure the decrease of an organic substrate (sodium acetate) in water by supplying oxygen in different modes, namely: (1) by feeding the membrane tube either with oxygen or air (or none of them); (2) in some cases by simultaneous sparging air to the residual water. The dynamics of the substrate and oxygen consumption were measured during the batch experiment, and two mathematical models are developed to predict their transient responses using a Monod kinetic with dual substrate limitation. The models predict biomass growth and the production of extracellular polymer substances (EPS), which in turn causes the biofilm to grow; they account for the counter-diffusion of substrate and oxygen within the EPS structure that contains the cells, and one of them incorporates the mass transport by convection and diffusion in the surrounding liquid contained inside the interconnected pores and channels within the biofilm. Transport and kinetic parameters are estimated from experiments, and both models successfully predict concentration measurements in some of the set of experiments. It was found that all of the modes of oxygen supplied in a MABR were more efficient than the traditional suspended cell process.     

Separation of Triacylglycerol Species from Interesterified Oils by High-Performance Liquid Chromatography

Using a 1,3-regioselective lipase as a catalyst, soybean oil and olive oil were interesterified with the short-chain triacylglycerol tributyrin (1,2,3-tributyrylglycerol) to produce mixtures of structured triacylglycerols (SL-TAG). The SL-TAG were purified by column chromatography and analyzed by both normal-phase (silica column; NP_SIL) and reversed-phase [octadecyl silane (ODS) column] high-performance liquid chromatography (HPLC). Individual SL-TAG molecular species were detected by evaporative light-scattering detection, and characterized by mass spectrometry. NP_SIL HPLC successfully separated the newly synthesized SL-TAG into two groups of TAG: one composed of one butyryl group and two long-chain fatty acyl groups (from soybean or olive oil); the second was composed of two butyryl groups and one long-chain fatty acyl group. The SL-TAG species were further analyzed by reversed-phase HPLC which gave a more detailed separation of the TAG species present in the two SL-TAG.     

Mass Balance Analysis of Ozone in a Conventional Bubble Column

Ozone transfer into potable water was studied in a conventional bubble column, and ozone mass balances have been calculated to determine ozone utilization efficiencies. Liquid and gas flow rates, as well as inlet ozone concentrations in the gas phase were varied. Using these data, it was possible to determine the ozone mass transfer coefficient, ozone transfer efficiency, and ozone consumption. A model of ozone transfer was established, and procedures for calculating the optimum design parameters and operating conditions are proposed.