Scale-up of protein purifications using aqueous two-phase systems: comparing multilayer toroidal coil chromatography with centrifugal partition chromatography

Two different laboratory scale liquid-liquid extraction processes using aqueous two-phase systems (ATPS) are compared: centrifugal partition chromatography (CPC) and multilayer toroidal coil chromatography (MTCC). Both use the same phase system, 12.5% (w/w) PEG-1000:12.5% (w/w) K(2)HPO(4), the same flow rate of 10 mL/min and a similar mean acceleration field of between 220 × g and 240 × g. The main performance difference between the two processes is that there is a continuous loss of stationary phase with CPC, while for MTCC there is not - even when sample loading is increased. Comparable separation efficiency is demonstrated using a mixture of lysozyme and myoglobin. A throughput of 0.14 g/h is possible with CPC despite having to refill the system with stationary phase before each injection. A higher throughput of 0.67 g/h is demonstrated with MTCC mainly due to its ability to tolerate serial sample injections which significantly reduces its cycle time. While CPC has already demonstrated that it can be scaled to pilot scale, MTCC has still to achieve this goal.     

两类多元GARCH模型的预测绩效和组合VaR的研究

运用V aR模型对股票组合进行风险测度的关键之一是得到组合条件协方差矩阵.而经典的多元GARCH模型来求解波动率面临着估计参数过多,计算量庞大的问题.因此,使用正交GARCH模型和CCC模型来估算波动率,并以沪深两市A股市场上四个行业的65只股票为样本,使用RM SE和M AD指标比较这些模型的预测能力,求得股票组合的V aR,得出前者效率高和后者预测能力略高的结论.     

When is a Pixley-Roy hyperspace CCC?

A space X is said to satisfy condition (C) if for every Y?X with |Y|=ω₁, any family $\text{G}$ of open subsets of Y with |$\text{G}$|=ω₁ has a countable network. It is easy to see that if X satisfies condition (C), then its Pixley-Roy hyperspace $\text{F}$[X] is CCC. We show that under MA_ω1 condition (C) is also necessary for $\text{F}$[X] to be CCC, but under CH it is not.     

Retention of fluorinated chiral selectors in biphasic fluorinated solvent systems and its application to the separation of enantiomers by countercurrent chromatography

Ethoxynonafluorobutane (ENFB) has been used as a component of new biphasic solvent mixtures. The suitability of several mixtures as solvent systems in countercurrent chromatography was tested. The applicability of the ENFB/2-PrOH/H₂O mixture to the separation of enantiomers, in combination with a fluorinated chiral selector (CS), was evaluated. N-Perfluoroundecanoyl-l-proline-3,5-dimethylanilide (2), analogous to the previously used N-dodecyl-l-proline-3,5-dimethylanilide (1), was synthesized for this purpose. The capacity of the new solvent system to retain the fluorinated CS in the fluorinated phase used as stationary was examined. Chiral selector 1 was applied in analogous conditions for comparative purposes. Additionally, MTBE/phosphate buffer solvent system was also used with the two CSs. The ENFB/2-PrOH/H₂O (25:35:40) mixture was found to be adequate in the enantioseparation of DNB-Leu and DNB-Leu-tBu. Enantioselectivity was maintained in the fluorinated solvent system without compromising eluting time. The complete separation of DNB-Leu-tBu was achieved and no leaks of CS to the mobile phase were detected.     

On cardinal invariants for CCC -ideals

We show several results about cardinal invariants for -ideals of the reals. In particular we show that for every CCC -ideal on the real line .

     

高效液相色谱-串联质谱法测定动物源性食品中矮壮素残留

建立了高效液相色谱-串联质谱测定动物源性食品中矮壮素残留的分析方法。样品经含1%(v/v)乙酸的乙腈溶液提取、正己烷脱脂、阳离子固相萃取柱(PCX)净化,采用Venusil MP C18(2)色谱柱(150 mm×2.1 mm, 3μm)分离,以乙腈和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,采用电喷雾电离、正离子模式扫描,多反应监测模式(MRM)检测,基质匹配标准曲线内标法定量。结果表明:矮壮素在0.200～500μg/L范围内呈良好线性,相关系数(r²)均不低于0.999 3,方法的定量限为0.500μg/kg;以猪肉、牛肉、羊肉、鸡肉、鸡蛋、猪肾、牛肝、羊肾、鸡肝、牛奶为基质,矮壮素的平均加标回收率为93.4%～101%,相对标准偏差为2.3%～8.0%。该方法基质干扰小,灵敏度高,准确可靠,适用于动物源性食品中矮壮素残留的定量检测。     

MECHANLCAL FAILURE IN HAVERSIAN SYSTEMS ON THE BASIS OF MICROSTRUCTURE

The aim of this paper is to observe variations in the mechanical properties of Haversian systems including Haversian lamellae and canals,by means of the compressive test of five bone specimens subjected to different loads corresponding to 2KN,3KN,dKN,5KN and 6KN respectively. From a series of related microscopic pictures it is clearly seen that:(1) in the lower level of loading (2KN) ,the Haversian canals much the same as the one unsubjected to loads,and conditions of Harversian lamellae are also the same,but,the individual Harversian canal was slightly bent; (2) in the case of the higher levels of loading,it is first deformed in the weaked portion of the Haversian lamellae; (3) with increasing loads,the fracture shapes of the Haversian system are very complex,but the fractures always take place in the cement line between osteons.At the same time,deformed dimensions of the Harversian lamellae and canals were measured. The observed phenomena were qualitatively interpreted by the theory of the linear viscoelas-ticity.     

同步逆流色谱仪固相保留分析

为了提高同步逆流色谱仪的固相保留率,扩大逆流色谱仪的应用范围,本文通过结合物理、数学知识,分析影响逆流色谱仪固相保留率的主要因素：固-液摩擦力、液-液摩擦力之间的相互影响,并且数学模型验证了平面螺旋柱的切向离心力作用,三者共同决定了流动相的在柱内流速的改变,从而影响到柱内流动相的横截面积,继而影响到固定相的横截面积,最终决定了固相保留率的大小,并通过实验结果加以验证,得出F-H-U与R-H-U另种模式的固相保留效果最好。     

Purification of high-throughput organic synthesis libraries by counter-current chromatography

Experiments were performed to evaluate whether counter-current chromatography (CCC) could function as an alternative purification method to reversed-phase high-performance liquid chromatography (RP-HPLC) and normal-phase supercritical fluid chromatography (SFC). RP-HPLC and SFC are the routine methods currently used in our high-throughput purification (HTP) facility for the purification of high-throughput organic synthesis (HTOS) libraries and medicinal chemistry reaction mixtures. Pre-equilibration of the solvent mixture layers was not mandatory for effective chromatography when hexanes–ethyl acetate–methanol–water (HEMW) solvent mixtures were used. Key to the use of CCC for high-throughput applications is the ability to effectively select a solvent system appropriate to each library member. Pilot-scale CCC elution time was used to estimate a starting solvent ratio and RP-HPLC retention time was then used to adjust solvent ratios within a particular library. It was also found that dimethyl sulfoxide (DMSO) and DMSO–methanol were suitable as sample injection solvents when using the HEMW solvent systems.