Predicting the selectivity of imprinted polymers

Summary Imprinted polymers as stationary phases for HPLC separations have been the subject of extensive investigations in recent years. In order to aid the rational design of synthetic protocols for the preparation of imprinted polymers, a series of calculations were made to assess the equilibrium concentration of templatemonomer complexes as a function of association constant (K) for the functional groups involved in the interactions and initial concentrations of reactants. This data was then used to predict the selectivity of polymers prepared under different reaction conditions and the model was tested using an experimentally determined value ofK and separation factors taken from the literature.     

套索冠醚毛细管色谱柱的研制

用套索冠醚N,N′-双(2-甲基吡啶)-二氮杂-18-冠-6作为固定相,涂渍在弹性石英毛细管内,测其柱效、惰性、热稳定性、平均极性及选择性等性质.其结构由元素分析、红外光谱、核磁共振及质谱分析的试验数据所证实.试验表明,它具有良好的色谱性能、中等极性,适用于对醇、卤代烃、芳香烃等各类异构体的分离,并用分子结构观点探讨了保留机理.     

Optimisation of chiral separation of omeprazole and one of its metabolites on immobilized α1-acid glycoprotein using chemometricsglycoprotein using chemometrics

Summary A strategy for the optimisation of direct chiral separation of omeprazole and a metabolite, hydroxi-omeprazole, in reversed phase liquid chromatography is described. A factorial design was used, where mobile phase pH, concentration of a mobile phase modifier, ionic strength and column temperature were tested as the variables and enantioselective retention, column efficiency and asymmetry factor as the responses. The experimental results were evaluated with multivariate analyses, which demonstrated that the column temperature and content of mobile phase acetonitrile were by far the most important variables. The enantiomers of omeprazole and one of its metabolites were baseline resolved within 15 minutes. The optimised chromatographic system was used for a separation of the enantiomers of omeprazole and its main metabolite in a patient plasma sample.     

分子筛改性气—液毛细管柱及其性能考察

以原位合成法制备的分子筛膜对玻璃毛细管内壁进行改性后，成功地制备了常规口径及大口径分配ＳＣＯＴ柱，并对毛细管柱的性能进行了评价。     

Mercury species immobilized on sulphydryl cotton: A new candidate reference material for mercury speciation

A batch of sulphydryl cotton microcolumns was prepared and charged with a mixed Hg standard solution (methyl-, ethyl- and inorganic Hg, 10 g l^–1 as Hg, 3 ml) and stored at 4 °C in a light-tight box. At regular time intervals over a 4 month period microcolumns were removed and Hg species were quantified by gas chromatography microwave-induced plasma atomic emission spectrometry (after elution, extraction and derivatization steps). It was found that analyte recoveries for methyl- and inorganic Hg were quantitative over the 4 month period while ethyl-Hg species appeared to be stable for up to 2 months.     

稀土—4—（2—吡啶偶氮）间苯二酚螯合物的高效液相色谱分离和测定

本文讨论了反相离子对液相色谱法分离和检测稀土-4-(2-吡啶偶氮)间苯二酚螯合物的各种条件,在12 min内完成了9种稀土螫合物的分离,校正曲线的线性范围是(ppm):La(0.01～3.20),Ce(0.03～2.8),Pr(0.06～3.5),Nd(0.05～3.8),Sm(0.01～3.0),Eu(0.05～3.4),Tb(0.02～3.0),Ho(0.01～3.4),Er(0.06～4.0).变异系数小于1.2％.     

Composition and major odorous compounds of the essential oil of Bifora radians,an aldehyde-producing weed

The composition of the essential oil of Bifora radians, an aldehyde-producing weed, has been investigated by capillary gas chromatography, coupled gas chromatography – mass spectrometry, on-line catalytic hydrogenation and coupled gas chromatography – infrared spectrometry. The nineteen compounds identified included eighteen aldehydes: seven alkanals (C6, C9, C10, C11, C12, C13, and C14), ten alkenals, including five (E)-2-alkenals (C12, C13, C14, C15, and C16), and one (E,E)-2,4-alkadienal (C13). Typical Bifora odors were attributed to three major (E)-2-alkenals, C12, C13, and C14.     

Determination of particulate fatty acids as P-bromophenacyl- or phenylphenacylesters using HPLC

Summary A method for the determination of fatty acids of the molecular weight range of propionic to erucic acid is reported. The acids are converted to either p-bromophenacyl-or p-phenylphenacylesters and the esters are separated by HPLC and detected by UV-absorption. Twentytwo esters, including saturated, monoolefinic and polyunsaturated ones were separated within one HPLC-run. The detection limit is about 5 pmol per fatty acid. The application of the method to particulate material is described.     

Chromatographic evaluation of perphenylcarbamoylated β-cyclodextrin bonded stationary phase for micro-high performance liquid chromatography and pressurized capillary electrochromatography

Application of mono (6^A-N-ethylenediamine-6^A-deoxy) perphenylcarbamoylated β-cyclodextrin (β-CD) bonded stationary phase (CSP) in micro-high performance liquid chromatography (micro-HPLC) and pressurized capillary electrochromatography (p-CEC) was firstly presented. A series of racemic α-amidophosphonates were resolved in reversed- and normal-phase modes on this CSP. The investigated chromatographic parameters include retention factor (k′), separation factor (α) and resolution (Rs) of solutes. In addition, the structural variation of the solutes and the experimental factors affecting chiral separations have been examined, including the percentage of alcohol modifier, the linear velocity (u) of the mobile phase, electrical field strength, etc. Baseline separation was achieved for most of the entities. Hydrophobic interaction, steric effect and π-π interaction contribute to the possible mechanism. Comparative results indicate that higher Rs value up to 3.1 was found in micro-HPLC, higher efficiency up to 29,970 in p-CEC.