Evaluation of dead time calculation in liquid chromatography using a linearization procedure for homologous series

A mathematical method for the calculation of the dead time (t_m) in HPLC was evaluated using a computer simulation approach, in which artificial perturbations were introduced to Simulated homolog retention times. The calculation was based on a modified and extended Grobler and Bálisz (GB) method. Investigated wav how the precision of the calculated t_M is affected by: statistical fluctuations in retention times and which, and how many homolog retention times are used. Based on these simulations a two-step procedure for the t_M calculation is proposed: In the first step the linearity of log t_{R, n} vs carbon number n is checked using as many homolog retention times as possible. The slope value b^o of the first linear regression in the GB method is used for the selection of homolog retention times in the final t_M calculation. In the second step the optimal selection of homologs is made and the final t_M calculation is carried out. Guidelines for homolog selection are given.     

Black fungus derived aerogel with double faced properties

Black fungus aerogel (BFA) exhibited interesting double-faced properties. Weexplored the diverse properties of each side of the black fungus in three aspects:water contact angle measurements, liquid selective absorption capacity and air pollutant adsorption abilities.     

Multilayer effects in liquid adsorption chromatography with mixed mobile phases

This paper describes the theory of liquid adsorption chromatography (LSC) with mixed mobile phase, involving formation of multilayer surface phases. An equation describing the dependence of the capacity ratio upon the mobile phase composition is derived and theoretical curves illustrating the same dependence are calculated accordingly by assuming different thicknesses of the surface phase.     

HPLC of antibiotics. 1. Streptolydigin and related compounds

Two new acyltetramic acids related to streptolydigin have been isolated from fermentations of Streptomyces lydicus. The principal members of this complex were resolved by TLC on silica gel. However, the methods of detection, permanganate spray or bioautography, were not suitable for both crude fermentation broths and purified extracts. Gas chromatography is unsuitable for the detection of either underivatized or silylated streptolydigins. High performance liquid chromatography (HPLC) particularly on triethylaminoethyl cellulose is rapid and sensitive and is the method of choice for the analysis of both crude and purified samples. Using high performance liquid chromatography, two components were detected in the complex, which are not observed using any of the other chromatographic procedures.     

色谱灰色数模的建立及其应用研究(Ⅰ)──连续GM(1,N)模型的建立及色谱保留行为的预测

应用灰色系统理论和最小二乘原理，推导出连续GM（1，N）模型，并将该模型用于高效液相色谱中溶质保留行为的预测．研究了烷烃、烷基苯及对羟基苯甲酸酯等化合物的容量因子与流动相组成、容量因子与碳数、保留时间与温度、保留时间与碳数的关系，并建立了相应的数学模型，经验证，预测结果良好．     

Isolation and determination of paspalitrem-type tremorgenic mycotoxins using liquid chromatography with diode-array detection

A liquid chromatographic (LC) method is described for the isolation and determination of the tremorgenic mycotoxins paxilline (Penicillium paxilli NRRL 6110), paspaline, paspalinine and paspalicine (Claviceps paspali). Following a Soxhlet extraction of a mould-contaminated matrix using chloroform, the crude extract was partitioned between hexane and 80% aqueous methanol. The latter fraction, containing the desired toxin(s), was evaporated to dryness, the residue dissolved in methylene chloride and the solution analysed by liquid chromatography using a Supelcosil LC-Si column eluted with methylene chloride-diethyl ether (9 + 1, v/v). A mixture containing standards of these compounds was similarly analysed. All toxins were detected using a UV diode-array detector. The generated UV spectra and chromatographic data of the standard toxins were stored in a computer as a library and used to identify these toxins in a crude mixture. The purity of the separated peaks and the amount of toxin in the crude mixture were also determined. The toxins were isolated by selectively collecting the eluted peaks using a programmable fraction collector equipped with a peak level sensor. Further confirmation of compound identity was achieved by mass spectrometry using the direct inlet probe method. In comparison with methods used previously to isolate these toxins, the present technique is fast and allows the acquisition of complete UV spectral information and chromatographic data and the isolation of multiple toxins in a single chromatographic operation.     

Unraveling the mystery of efficacy in Chinese medicine formula: New approaches and technologies for research on pharmacodynamic substances

Traditional Chinese medicine (TCM) is the key to unlock treasures of Chinese civilization. TCM and its compound play a beneficial role in medical activities to cure diseases, especially in major public health events such as novel coronavirus epidemics across the globe. The chemical composition in Chinese medicine formula is complex and diverse, but their effective substances resemble “mystery boxes”. Revealing their active ingredients and their mechanisms of action has become focal point and difficulty of research for herbalists. Although the existing research methods are numerous and constantly updated iteratively, there is remain a lack of prospective reviews. Hence, this paper provides a comprehensive account of existing new approaches and technologies based on previous studies with an in vitro to in vivo perspective. In addition, the bottlenecks of studies on Chinese medicine formula effective substances are also revealed. Especially, we look ahead to new perspectives, technologies and applications for its future development. This work reviews based on new perspectives to open horizons for the future research. Consequently, herbal compounding pharmaceutical substances study should carry on the essence of TCM while pursuing innovations in the field.     

Multifunctionality in spin crossover materials

One of the most important trends in the spin crossover (SCO) field is focused on the synthesis of new molecule-based functional materials in which the SCO properties may be combined with other physical or chemical properties in a synergic fashion. The current stage of investigations regarding interplay and synergic effects between SCO, magnetic coupling, liquid crystalline properties, host-guest interactions, non-linear optical properties, electrical conductivity, and ligand isomerization is highlighted and discussed.     

含X-型液晶基元的液晶高分子的研究

以4,4′-(烷撑二酰氧)二苯甲酰氯和2,5-二羟基-1,4-苯撑双-(对乙氧基苯甲酸酯)为单体,采用低温缩聚方法,合成了含X-型液晶基元和不同柔性链长度的主链型液晶聚合物。聚合物的液晶行为用DSC、偏光显微镜和X-光衍射进行了表征。对于样品升温消光后又重新出现双折射的异常现象,初步认为是加热过程中分子量提高的结果。     

Online photocatalytic device for highly selective pre-column fluorescence derivatization of 5-hydroxyindoles with benzylamine

A fluorimetric liquid chromatographic method for the determination of 5-hydroxyindoles based on the benzylamine derivatization process mediated through an online photocatalytic oxidation has been developed. In this study, we used a photocatalytic column comprising tefzel tubing packed with TiO₂-coated glass beads, as a pre-column derivatization reactor. The fluorescence derivatization of 5-hydroxyindoles using benzylamine proceeded during their passage through the reaction column under near-UV irradiation. The 5-hydroxyindole derivatives were separated continuously on a reversed-phase liquid chromatography within 50 min, using 100 mM acetate buffer (pH 4.6)-acetonitrile (72:28, v/v; isocratic elution) containing 3 mM sodium octanesulfonate; the samples were detected fluorimetrically at 465 nm upon excitation at 350 nm. The detection limits (signal-to-noise ratio = 3) of the 5-hydroxyindoles were in the range from 160 to 360 fmol per 5 μL injection. We have applied this method, which requires minimal sample pre-treatment, to the determination of 5-hydroxyindole-3-acetic acid in human urine.