HPLC separation of positional isomers on a dodecylamine-N, N-dimethylenephosphonic acid modified zirconia stationary phase

The chromatographic performance of a new zirconia stationary phase (DPZ) modified with dodecylamine-N,N-dimethylenephosphonic acid (DDPA) is studied by using positional isomers as probes. The DDPA modified zirconia via one phosphonic group has a polar inner-layer and a non-polar outer-layer on its surface. The alkyl chain of outer-layer provides the hydrophobic interaction, while the polar inner-layer that consists of an amine group and a free phosphonic group provided dipolar and ion-exchange/columbic repellent interaction sites. The effects of methanol content, ionic strength and pH of mobile phase on capacity factors of the solutes are studied in detail, and baseline separations of toluidine, nitroaniline, aminophenol, dihydroxybenzene, and nitrophenol isomers were achieved on the new zirconia stationary phase. In addition, retention mechanism of the isomers on the DDPA-modified zirconia stationary phase is also proposed.     

基于可移动中子源的瞬发γ活化成像研究进展

瞬发γ活化成像技术基于瞬发γ射线中子活化分析,结合准直测量或者伴随粒子测量手段,以实现对样品内部中元素位置分布的测量。当前大多数相关研究都是基于大型中子源开展的,这限制了该技术的应用场景,可移动小型化中子源是该技术现场应用的必然要求。基于可移动中子源的瞬发伽马活化成像技术按照准直方式可分为基于单孔准直、编码孔准直及伴随粒子测量三类,本文对其技术原理、研究进展及仍存在的问题进行介绍与讨论。目前的技术在空间分辨率上还需要进一步提升,未来将进一步结合图像处理算法提高成像质量并降低测量时间。     

Simultaneous separation of sixteen positional and optical isomers of the tryptophan family by ligand-exchange micellar electrokinetic chromatography

Summary Ligand-exchange micellar electrokinetic chromatography has been used for the simultaneous separation of 16 positional and optical isomers of the tryptophan family. The Cu(II) complex with L-hydroxyproline was used as the chiral selector. Two groups of anionic surfactant, linear alkylbenzenesulfonates (LAS) and straight-chain alkyl sulfates such as sodiumn-decyl sulfate (SDeS), sodium dodecyl sulfate (SDS) and sodiumn-tetradecyl sulfate (STS), were used for simultaneous separation. The best result was obtained by use of SDS. The influence of SDS concentration and of pH on the separation was investigated. The separation behavior in the absence of the Cu(II) complex with L-hydroxyproline was also examined. Use of organic modifiers causes the resolution to decrease. Relationships between the logarithm of the octanol-water partition coefficient (logP _OW) and resolution, and between logP _OW and migration time are discussed.     

Separation of positional isomers of mono-poly(ethylene glycol)-modified octreotides by reversed-phase high-performance liquid chromatography

The purpose of this study was to develop a reversed-phase high-performance liquid chromatographic method (RP-HPLC) for separating each positional isomer from low- to high-molecular-weight mono-PEGylated octreotides prepared by polyethylene glycol (PEG) derivatives with various molecular weights (2, 5, or 20 kDa). In the gradient elution using acetonitrile and 10 mM phosphate buffer at pH 7.0 on a Phenomenex Gemini C-18 column (250 mm × 4.6 mm id, 5 μm), each positional isomer of the mono-PEGylated octreotides was completely resolved with good resolution (PEG-2K: 7.6, PEG-5K: 6.6, and PEG-20K: 3.1). The optimal RP-HPLC condition also resolved the degradation products of mono-PEG-octreotide isomers in thermal stability studies at 55 °C and enzymatic stability studies with trypsin. In conclusion, the developed RP-HPLC method will be valuable for studying the effect of PEGylation site and the attached PEG size on the physicochemical and pharmacological properties of PEGylated octreotides.     

Single-machine scheduling with positional due indices and positional deadlines

In this paper, we study single-machine scheduling problems with due dates, positional due indices, deadlines and positional deadlines. The scheduling criteria studied in this paper include the number of position-violated tasks, the weighted number of position-violated tasks, and the maximum positional lateness of tasks, by also combining with other traditional scheduling criteria. For each problem, we either provide a polynomial-time algorithm or present an NP-hardness proof.     

PSBH中的组合优化问题及其计算方法

本文介绍了具有部分位置信息的SBH杂交测序（Positional Sequencing by Hy-bridization,简称PSBH）实验所产生的一个重构DNA片断的组合优化问题,并讨论了该问题最优重构的计算问题.通过对PSBH提供的谱集及其位置信息的分析处理,我们获得了若干判定最优重构片断头尾的分支定界准则以及确定其非头尾位置最可能出现k-tuple的动态规划计算方法,并由此给出了该PSBH问题的一个新重构算法.该算法允许PSBH谱集含有一般杂交实验中常常可能出现探针错配所产生的正错误,并且仅仅假设PSBH的谱集、位置信息和位置长度是已知的,所以我们的算法具有更一般的适应性和实用性.此外,由于我们给出的算法能够极大地利用PSBH的谱集和位置信息所蕴含的信息确定最优重构片断头尾及其中间位置最可能出现的k-tuple,极大地减少了PSBH重构中的随意性,所以我们的算法也是有效的,模拟PSBH实验的计算结果验证了这一点.     

杯[4]芳烃衍生物气相色谱固定相分离芳烃异构体的热力学/超热力学研究

用热力学／超热力学方法对杯[4]芳烃衍生物气相色谱固定相上芳烃位置异构体的分离进行了研究。考察了一系列芳烃位置异构体在杯芳色谱柱上分离过程的热力学参数及其选择性之间的关系,并对杯[4]芳烃衍生物气相色 谱固定相分离芳烃位置异构体的保留机理进行了探讨。     

Composition analysis of positional isomers of phosphatidylinositol by high-performance liquid chromatography

An HPLC-based method has been developed for composition analysis of six positional isomers of phosphatidylinositol (PI), of which the phosphatidyl group was connected to different positions of the myo-inositol moiety. The method employed a combination of two types of HPLC analyses. One was direct separation of the six PI isomers into four peaks of 1(3)-PI, 2-PI, 4(6)-PI and 5-PI on a normal-phase silica gel column. The second method was for the separations of 1-PI from 3-PI and 4-PI from 6-PI, which were not separable on the normal-phase column. This method involved conversion of PI isomers into pentakis-(R)-1-phenylethylcarbamate (PEC) derivatives, which were separated on a reversed-phase column. Using the established method, positional specificity of several engineered phospholipases D in enzymatic synthesis of PI from myo-inositol and phosphatidylcholine was investigated. This was performed by analyzing the isomeric composition of PIs synthesized by the mutant enzymes. Among five mutant enzymes tested, two showed strong specificity to 1-OH, one showed moderate preference to 1-OH, one preferred 3-OH, and one showed broad specificity towards 1-, 3-, 4- and 6-OH.     

The separation and determination of nitrophenol isomers by high-performance capillary zone electrophoresis

o-Nitrophenol, m-nitrophenol, and p-nitrophenol could well be separated by capillary zone electrophoresis (CZE) by only adjusting the run buffer with methanol. Efficiency up to 10⁵ theoretical plates per meter was achieved. The effects of several important factors were investigated to find optimum conditions. The linear range, regression equation, and the recovery were given. This method possessed the advantages of simplicity, rapidity, and good reproducibility; it can be developed for the separation of practical samples in environment analysis.