Overloaded elution band profiles of ionizable compounds in reversed‐phase liquid chromatography: Influence of the competition between the neutral and the ionic species

The parameters that affect the shape of the band profiles of acido‐basic compounds under moderately overloaded conditions (sample size less than 500 nmol for a conventional column) in RPLC are discussed. Only analytes that have a single pK_a are considered. In the buffer mobile phase used for their elution, their dissociation may, under certain conditions, cause a significant pH perturbation during the passage of the band. Two consecutive injections (3.3 and 10 μL) of each one of three sample solutions (0.5, 5, and 50 mM) of ten compounds were injected on five C₁₈‐bonded packing materials, including the 5 μm Xterra‐C₁₈ (121 Å), 5 μm Gemini‐C₁₈ (110 Å), 5 μm Luna‐C₁₈(2) (93 Å), 3.5 μm Extend‐C₁₈ (80 Å), and 2.7 μm Halo‐C₁₈ (90 Å). The mobile phase was an aqueous solution of methanol buffered at a constant _W^WpH of 6, with a phosphate buffer. The total concentration of the phosphate groups was constant at 50 mM. The methanol concentration was adjusted to keep all the retention factors between 1 and 10. The compounds injected were phenol, caffeine, 3‐phenyl 1‐propanol, 2‐phenyl butyric acid, amphetamine, aniline, benzylamine, p‐toluidine, procainamidium chloride, and propranololium chloride. Depending on the relative values of the analyte pK_a and the buffer solution pH, these analytes elute as the neutral, the cationic, or the anionic species. The influence of structural parameters such as the charge, the size, and the hydrophobicity of the analytes on the shape of its overloaded band profile is discussed. Simple but general rules predict these shapes. An original adsorption model is proposed that accounts for the unusual peak shapes observed when the analyte is partially dissociated in the buffer solution during its elution.     

光纤复合型油气井下压力温度测量系统

针对目前广泛使用的电子式油气井下压力温度测量系统可靠性低、高温环境漂移大的不足,设计了一种基于非本征型F-P干涉仪(EFPI)和光纤布喇格光栅(FBG)的复合型油气井下压力、温度测量系统,详细说明了其工作原理、传感器组成和信号解调方法,初步试验结果表明,该测量系统不仅克服了电子测量方式的不足,而且具有复用性好、测量精度高等优点.     

Immobilized polysiloxanes as stationary phases for high-performance liquid chromatography and solid phase extraction

Polysiloxanes immobilized onto the surfaces of porous silica particles have proven to be good stationary phases for the separation of multiresidues of pesticides and their metabolic/degradation products by reversed-phase high-performance liquid chromatography (RP-HPLC). Similar materials have proven effective for pre-concentration and clean-up procedures using solid phase extraction. The present paper describes the preparation and some applications of several of these packing materials.     

Operating Parameters Optimization of Buffer Gas in Optically Pumped Submillimeter Wave Laser

Based on the basic theory of molecular vibration relaxation and semi-classical density matrix theory, operating parameters optimization of buffer gas in the process of miniature pulsed optically pumped submillimeter wave laser was systemically studied and the theoretical calculated result was tested by experiments. The result would do favor to develop and study high-power and wide-range tunable miniature and high-efficient pulsed optically pumped submillimeter wave laser and also had some instruction to its application.     

Headspace SPME–GC Method for Acetone Analysis and its Biomedical Application

A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions the fiber was used for the analysis of acetone in human urine.     

微尺度效应对螺旋槽干气密封性能的影响

本文引用考虑微尺度效应的雷诺方程,推导出了考虑微尺度效应的螺旋槽干气密封内部流动的近似算法。应用本文提供的算法对文献中干气密封的不同实验工况进行了计算,与相应的实验数据对比,计算结果和实验结果基本符合;切向动量调节系数σv对计算结果在尺度越小时影响越大;考虑微尺度效应时开启力的计算结果更趋于实验数据。     

Thermodynamic Limit and Proof of Condensation for Trapped Bosons

We study condensation of trapped bosons in the limit when the number of particles tends to infinity. For the noninteracting gas we prove that there is no phase transition in any dimension, but in any dimension, at any temperature the system is 100% condensated into the one-particle ground state. In the case of an interacting gas we show that for a family of suitably scaled pair interactions, the Gross–Pitaevskii scaling included, a less-than-100% condensation into a single-particle eigenstate, which may depend on the interaction strength, persists at all temperatures.     

淋洗液发生器离子色谱抑制电导法测定甜味剂

采用淋洗液发生器阴离子交换-抑制电导检测法,同时分离和检测阿思巴甜、甜蜜素、安赛蜜和糖精4种常见的甜味剂.由于采用了淋洗液发生器,使背景电导大大降低,可以实现甜味剂的高灵敏度检测和分离.该方法具有良好的重现性、线性关系和较低的检测限.阿思巴甜、甜蜜素、安赛蜜和糖精的检测限分别是:1.27、0.045、0.033、0.063 mg/L;样品测定的回收率分别为99.7%、102.8%、98.6%、103.5%.     

Optimized Method for the Determination of Prednisolone, Zn-Bacitracin and Phenylephrine in Local Pharmaceutical Preparations by Micellar Electrokinetic Capillary Chromatography

Summary A new, rapid and simple method is described and applied to resolve and quantify mixtures of prednisolone, Zn-bacitracin and phenylephrine. The determination was accomplished by MEKC. The separation was carried out at 25 °C and 30 kV, using a 5 mM phosphate-5 mM borate buffer (pH=8.2), 40 mM SDS as background electrolyte. Under these conditions, the run time was 6.6 min and the limits of quantification were about 1.0 mg L^–1 for every component. Repeatability and reproducibility studies were achieved showing no significant differences at 95% confidence level. The MEKC method has been applied for quantifying these compounds in different commercials pharmaceuticals products, without separations steps.