Micellar electrokinetic capillary surfactants

High-efficiency separations of FQ-labeled proteins are only achieved in the presence of an anionic surfactant, such as SDS. As a result, capillary isoelectric focusing is not useful for the analysis of these proteins. Instead, we employ capillary sieving electrophoresis and micellar electrokinetic capillary chromatography for our two-dimensional electrophoresis. 

Table 4.25 Surfactants used in micellar electrokinetic capillary chromatography...

Micellar electrokinetic capillary chromatography (MEKC or MECC) is a more versatile technique than CZE due to its ability to separate neutral as well as ionic species. The term chromatography is used because a surfactant added to the buffer solution forms spherical aggregates of molecules... 

In order to separate neutral compounds, Terabe et al. [13] added surfactants to the buffer electrolyte. Above their critical micellar concentration (cmc), these surfactants form micelles in the aqueous solution of the buffer electrolyte. The technique is then called Micellar electrokinetic capillary chromatography, abbreviated as MECC or MEKC. Micelles are dynamic structures consisting of aggregates of surfactant molecules. They are highly hydrophobic in their inner structure and hydrophilic at the outer part. The micelles are usually... 

The next important milestone in CE was achieved in 1984, when Terabe et al. described the method of micellar electrokinetic capillary chromatography (MECC or MEKC). By simply adding a surfactant to the separation buffer electrolyte, it was possible to separate both charged and neutral compounds simultaneously in CE. Erom this point on, the technique developed rapidly with many applications resulting in a demand for identification information. Coupling of CE to mass spectrometry was a next challenge and the... 

Micellar electrokinetic capillary chromatography (MECC), in contrast to capillary electrophoresis (CE) and capillary zone electrophoresis (CZE), is useful for the separation of neutral and partially charged species [266,267]. In MECC, a surfactant, usually sodium dodecyl sulfate (SDS), is added to the buffer solution above its critical micellar concentration to form micelles. Although SDS is certainly the most popular anionic surfactant in MECC, other surfactants such as bile salts have proved to be very effective in separating nonpolar analytes that could not be resolved using SDS [268]. 

If pH does not provide adequate separation or if analytes are neutral, use surfactants for micellar electrokinetic capillary chromatography. For chiral solutes, try adding cyclodextrins. 

Micellar electrokinetic chromatography (MEKC) is a modality of liquid chromatography having a surfactant molecule in the form of a micelle, which was introduced by Terabe et al. in 1984 [38]. The formation and separation occur in the capillary and, hence, it is also called micellar electrokinetic capillary chromatography (MECC). This modality is useful for some specific molecules having solubilities in micelles and, therefore, utilized for the separation and identification of such compounds with great efficiency, reproducibility, and low levels of detections. The most commonly used compounds for micelle formation are sodium dodecyl sulfate (SDS), sodium tetradecyl sulfate, sodium decanesulfonate, sodium /V-lauryl-/V-mcthyllauratc, sodium... 

Many pharmaceutical preparations contain multiple components with a wide array of physico-chemical properties. Although CZE is a very effective means of separation for ionic species, an additional selectivity factor is required to discriminate neutral analytes in CE. Terabe first introduced the concept of micellar electrokinetic capillary chromatography (MEKC) in which ionic surfactants were included in the running buffer at a concentration above the critical micelle concentration (CMC) [17], Micelles, which have hydrophobic interiors and anionic exteriors, serve as a pseudostation-ary phase, which is pumped electrophoretically. Separations are based on the differential association of analytes with the micelle. Interactions between the analyte and micelles may be due to any one or a combination of the following electrostatic interactions, hydrogen bonding, and/or hydro-phobic interactions. The applicability of MEKC is limited in some cases to small molecules and peptides due to the physical size of macromolecules... 

Micellar electrokinetic capillary chromatography (MECC) is a mode of CE similar to CZE, in which surfactants (micelles) are added to the buffer system. Micellar solutions can be used to solubilize hydrophobic compounds that would otherwise be insoluble in water. In MECC the micelles are used to provide a reversed-phase character to the separation mechanism. Although MECC was originally developed for the separation of neutral species by capillary electrophoresis, it has also been shown to enhance resolution in the analysis of a variety of charged species.16... 

Table 5.3 Typical Surfactant Systems Used in Micellar Electrokinetic Capillary Chromatography...

Enormous advances and growth in the use of ordered media (that is, surfactant normal and reversed micelles, surfactant vesicles, and cyclodextrins) have occurred in the past decade, particularly in their chromatographic applications. New techniques developed in this field include micellar liquid chromatography, micellar-enhanced ultrafiltration, micellar electrokinetic capillary chromatography, and extraction of bioproducts with reversed micelles techniques previously developed include cyclodextrins as stationary and mobile-phase components in chromatography. The symposium upon which this book was based was the first major symposium devoted to this topic and was organized to present the current state of the art in this rapidly expanding field. 

The first reports of micellar electrokinetic capillary chromatography (MECC or MEKC) appeared in the literature in 1984 [16]. Through April 2002, there have been over 1100 English-language papers published in the field. The subject is covered in all general textbooks on capillary electrophoresis. While a vast number of surfactants and related reagents can be employed, most separations can be accomplished with a few simple recipes. 

Crosby D, El Rassi Z. Micellar electrokinetic capillary chromatography with cationic surfactants. J Liq Chromatogr 1993 16 2161. 

Mechref, Y. El Rassi, Z. Micellar electrokinetic capillary J chromatography with in-situ charged micelles VI. Eval- Q uation of novel chiral micelles consisting of steroidal- glycoside surfactant-borate complexes. J. Chromatogr., A S... 

Micelles and cyclodextrins are the most common reagents used for this technique. Micellar electrokinetic capillary chromatography (MECC or MEKC) is generally used for the separation of small molecules [6], Sodium dodecyl sulfate at concentrations from 20 to 150 mM in conjunction with 20 mM borate buffer (pH 9.3) or phosphate buffer (pH 7.0) represent the most common operating conditions. The mechanism of separation is related to reversed-phase liquid chromatography, at least for neutral solutes. Organic solvents such as 5-20% methanol or acetonitrile are useful to modify selectivity when there is too much retention in the system. Alternative surfactants such as bile salts (sodium cholate), cationic surfactants (cetyltrimethy-lammonium bromide), nonionic surfactants (poly-oxyethylene-23-lauryl ether), and alkyl glucosides can be used as well. 

Micellar Electrokinetic Capillary Chromatography. Surfactants that form micelles in solution are added to the buffer in the capillary. When the solute is injected, it partitions itself between the buffer and the micelle. Migration of the solute depends on the amount of time it spends in the micelle versus the time it spends in the buffer. Therefore, the separation of analytes occurs due to differences in the partition coefficient between the two phases, much like in a chromatographic process. 

Micellar electrokinetic capillary chromatography (MEKC) is used, often, for separating neutral and hydrophobic molecules. The surfactants in MEKC have the added advantage of solubilizing proteins. This can eliminate the need for extraction or deproteinization, allowing direct sample injection. The effect of sample matrix in MEKC is less dramatic than that in CZE. A... 

Micellar electrokinetic capillary chromatography uses a totally aqueous buffer into which a surfactant in excess of its critical micelle concentration is introduced [18,35—37]. This approach makes use of solute separation via partitioning into... 

A micellar electrokinetic capillary chromatographic (MECC) method to separate 17 dihydroergotoxines, aci-alkaloids, and oxidation products has been described [103]. The authors used novel cationic dimeric (Gemini) surfactants such as l,3-bis(dodecyl-W,N-dimethyl ammonium)-2-propanol and l,3-bis(te-tradecyl-N,N-dimethyl ammonium)-2-propanol for the separation in less than 8 min. 

C.-E. Lin, C.-C. Hsueh, T.-Z. Wang, T.-C. Chiu and Y.-C. Chen, Migration behavior and separation of s-triazines in micellar electrokinetic capillary chromatography using a cationic surfactant,... 

C. Fujimoto, Y. Fujise and S. Kawaguchi, Macromolecular surfactant as a pseudo-stationary phase in micellar electrokinetic capillary chromatography, J. Chromatogr. A, 871, 415-425, 2000. 

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