Phase separation detection

Phase separation detectable at a nanometer scale (Newman et al. 2008 Lauer et al. 2011) Amorphous mixtures and strong drug-polymer interactions require the components in the system to be in close spatial proximity, which can be detected by SS-NMR... 

Phase Separation Detection by Atomic Force Microscopy... 

SFIG or SFG from a medium that has a strong response in a separate detection anu. By this means, one may fiilly compensate for variations not only in pulse energy, but also in the temporal and spatial substructure of the laser pulses. Some experiments may require measurement of the phase of the nonlinear signal [57]. 

For more specific analysis, chromatographic methods have been developed. Using reverse-phase columns and uv detection, hplc methods have been appHed to the analysis of nicotinic acid and nicotinamide in biological fluids such as blood and urine and in foods such as coffee and meat. Derivatization techniques have also been employed to improve sensitivity (55). For example, the reaction of nicotinic amide with DCCI (AT-dicyclohexyl-0-methoxycoumarin-4-yl)methyl isourea to yield the fluorescent coumarin ester has been reported (56). After separation on a reversed-phase column, detection limits of 10 pmol for nicotinic acid have been reported (57). 

A sensitive determination of alkanesulfonates combines RP-HPLC with an on-line derivatization procedure using fluorescent ion pairs followed by an online sandwich-type phase separation with chloroform as the solvent. The ion pairs are detected by fluorescence. With l-cyano-[2-(2-trimethylammonio)-ethyl]benz(/)isoindole as a fluorescent cationic dye a quantification limit for anionic surfactants including alkanesulfonates of less than 1 pg/L per compound for a 2.5-L water sample is established [30,31]. 

The ion pair extraction by flow injection analysis (FIA) has been used to analyze sodium dodecyl sulfate and sodium dodecyl ether (3 EO) sulfate among other anionic surfactants. The solvating agent was methanol and the phase-separating system was designed with a PTFE porous membrane permeable to chloroform but impermeable to the aqueous solution. The method is applicable to concentrations up to 1.25 mM with a detection limit of 15 pM [304]. 

Chloropromazine (8—34 wt% loading) has been microencapsulated in PCL-cellulose propionate blends by the emulsion solvent evaporation method (61). Phase separation for some ratios of the two polymers was detectable by SEM. The release rate from microcapsules in the size range of 180-250 pm in vitro (Fig. 11) was directly proportional to the PCL content of the blend, the half-life (50% drug release)... 

In the case of precipitation by monovalent salts (NaCl), the phase separation was taken at the initial break points in the resulting optical density versus NaCl concentration curves obtained at 600 nm. This method has been also used to detect the phase separation with CuCl2 at very low polymer concentrations. 

Since spillover phenomena have been most directly sensed through the use of IR in OH-OD exchange [10] (in addition, in the case of reactions of solids, to phase modification), we used this technique to correlate with the catalytic results. One of the expected results of the action of Hjp is the enhancement of the number of Bronsted sites. FTIR analysis of adsorbed pyridine was then used to determine the relative amounts of the various kinds of acidic sites present. Isotopic exchange (OH-OD) experiments, followed by FTIR measurements, were used to obtain direct evidence of the spillover phenomena. This technique has already been successfully used for this purpose in other systems like Pt mixed or supported on silica, alumina or zeolites [10]. Conner et al. [11] and Roland et al. [12], employed FTIR to follow the deuterium spillover in systems where the source and the acceptor of Hjp were physically distinct phases, separated by a distance of several millimeters. In both cases, a gradient of deuterium concentration as a function of the distance to the source was observed and the zone where deuterium was detected extended with time. If spillover phenomena had not been involved, a gradientless exchange should have been observed. 

The degree of conversion of the reactant and the concentration of oxidised products were carefully monitored by HPLC analysis. Sample components were separated on an ion-exchange column (Sarasep Car-H, 300mm x 7.8mm i.d.) using a 0.0004M H2SO4 mobile phase and detected by UV and RI detectors mounted in series. 

Silicon is separated on silica gel layer using light petroleum + diethyl ether (98 2) as the mobile phase and detection with rhodamine B... 

Figure 7.9 A, ScheMtic representation of cosplex fomtlon between an anlno acid and copper in the presence of a diysically inaobllized chiral selector. B, separation of D-leu-L-leu(l) and L-leu-D-leu(2) on a CHIR plate with aethanol-propan-l-ol-vater (5 1 4) as the mobile phase with detection at 410 na. (Reproduced with permission from ref. 109. Copyright Dr. Alfred Huethig Publishers).

No turbidity has been detected in the concentration ranges investigated. However the reduced viscosity i/red is a decreasing fonction of Ca at pH 5 and pH 7. This result shows that this polymer interacts with aluminium although no phase separation has been observed. 

Recently, due to increased interest in membrane raft domains, extensive attention has been paid to the cholesterol-dependent liquid-ordered phase in the membrane (Subczynski and Kusumi 2003). The pulse EPR spin-labeling DOT method detected two coexisting phases in the DMPC/cholesterol membranes the liquid-ordered and the liquid-disordered domains above the phase-transition temperature (Subczynski et al. 2007b). However, using the same method for DMPC/lutein (zeaxanthin) membranes, only the liquid-ordered-like phase was detected above the phase-transition temperature (Widomska, Wisniewska, and Subczynski, unpublished data). No significant differences were found in the effects of lutein and zeaxanthin on the lateral organization of lipid bilayer membranes. We can conclude that lutein and zeaxanthin—macular xanthophylls that parallel cholesterol in its function as a regulator of both membrane fluidity and hydrophobicity—cannot parallel the ability of cholesterol to induce liquid-ordered-disordered phase separation. 

Toll, H., Oberacher, H., Swart, R., Huber, C.G. (2005). Separation, detection, and identification of peptides by ion-pair reversed-phase high-performance hquid... 

Electrospray ionization (ESI) is ideally suited as a detection technique for the online interfacing of liquid-phase separations (HPLC and CE) to MS, because it facilitates the transfer of analytes from the liquid phase of the HPLC or CE column to the gas phase of the MS. Also, it allows the detection of high molecular weight species, such as peptides. Three interface designs have been developed in the past 18 years for coupling CE with MS. The first CE-MS interface, coaxial sheath flow, was introduced by Smith and his group in 1987 (Olivares et al., 1987) and was improved upon in later work (Smith et al., 1988). Coaxial sheath flow is formed using two concentric metal capillaries, whereby the CE terminus and the makeup flow line are inserted into the... 

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