Columns ethanolamines

A) 1-(2-Amino-5-chlorophenyll-1-(2-fluorophenyll-2-a2a-but-1-en-4-ol A mixture of 40 g of 2-methylimidazole hydrochloride and of 90 g of 2-amino-5-chloro-2 -fluoro-benzophenone in 240 ml of ethanolamine is heated at 135 for 2 hours. After cooling, the reaction mixture is poured into an aqueous sodium bicarbonate solution. The mixture is extracted with ether, the organic phase is washed repeatedly with water and is dried over sodium sulfate, and the solvent is evaporated to dryness. The residual oil is chromatographed on a silica column, elution being carried out with a 50/50 mixture of cyclohexane and ethyl acetate. 

The polyamines putrescine, cadaverine, spermidine, and spermine, which are seen at elevated levels in some victims of cancer, were separated on a Technicon (The Technicon Company Chauncey, NY) TSM Amino Acid Analyzer packed with an 8% divinylbenzene-co-polystyrene sulfonated resin with post-column ninhydrin detection.111 Amines such as ethanolamine, noradrenaline, hexamethylene diamine, methoxytryptamine, spermine, and spermidine were separated from amino acids on a DC-4A cation exchange resin.112 A similar approach, using a Beckman Model 121M amino acid analyzer equipped with an AA-20 column, was also successful.113 A Polyamin-pak strong cation exchange column (JASCO) was eluted with a citrate buffer for the detection of putrescene, spermine, cadaverine, and 1,5-diaminohex-ane from rat thymus.114 A post-column o-phthaldehyde detection system was used. 

A packed column is used to absorb S02 from flue gas using an ethanolamine solution. The column is 4 ft in diameter, has a packed height of 20 ft, and is... 

Figure 22 Dynamics of principal lipid constituents in horse-mackerel during cruising and fatigue. (After Yuneva et al., 1991.) The free fatty-acid level increases in red muscle and liver when the fish swim, and decreases during fatigue. Other constituents decrease under both conditions. TG, triacyl-glycerols PL, phospholipids PC, phosphatidyl choline PE, phosphatidyl ethanolamine FFA, free (unesterified) fatty acids. Black columns, red muscle empty columns, white muscle shaded, liver.

Higher ammonia-ethylene oxide ratios favor high yields of diethanolamine and triethanolamine, whereas lower ratios are used where maximum production of monoethanolamine is desired. The reaction is noncatalytic. The pressure is moderate, just sufficient to prevent vaporization of components in the reactor. The bulk of the water produced in the reaction is removed by subsequent evaporation. The dehydrated ethanolamines then proceed to a further drying column, after which they are separated in a series of fractionating columns, not difficult because of the comparatively wide separation of their boiling points. 

Commercial production of ethanolamines (EOA) is by reaction of ethylene oxide with aqueous ammonia. The ethylene oxide reacts exothermically with 20% to 30% aqueous ammonia at 60 to 150°C and 30 to 150 bar in a tubular reactor to form the three possible ethanolamines (mono-ethanolamine - MEA, di-ethanolamine - DEA and tri-ethanolamine - TEA) with high selectivity. The product stream is then cooled before entering the first distillation column where any excess ammonia is removed overhead and recycled. In the second column, ammonia and water are removed and the EOA s are separated in a series of vacuum distillation columns. 

As described earlier, the total cellular lipids can be recovered by use of a neutral organic solvent system, such as chloroform-methanol-water. Silicic acid column chromatography, thin-layer chromatography, and high-pressure liquid chromatography (HPLC) are well suited to isolation of the ethanolamine-rich phospholipids. Only column and thin-layer chromatographic purification will be discussed at this juncture. 

Of halogenated acetyl derivatives, trifluoroacetyl derivatives are mainly used for the sensitive analysis of amines, particularly owing to their better chromatographic properties despite their ECD response being lower than that of chloroacetyl derivatives (cf., Table 4.7, p. 69). Trifluoroacetyl derivatives were exploited for the GC separation of a mixture of saturated and unsaturated homologues of amines up to C22 on conventional packed columns [71]. Mori et al. [72] developed a method for the quantitative and qualitative GC analysis of m- and p-xylenediamines in polyamides in the form of their t N -trifluoro-acetyl derivatives. An analogous method was elaborated for the analysis of ethanolamine for the presence of mono-, di- and triethanolamine [73]. A 1-ml volume of TFA anhydride is stoppered in a 2-ml vial, which is evacuated with the aid of a 10-ml injection syringe. 

Fig. 5.8. Gas chromatogram of a mixture of 2,4-dinitrophenyl derivatives of amines. Peaks 1 = ammonia 2 = diethylamine 3 = isopropylamine 4 = rm.-butylamine 5 = sec.-butylamine 6 = iso-amylamine 7 = n-amylamine 8 = TMS-ethanolamine 9 = aniline 10 = cyclohexylamine 11 = benzyl-amine 12 = (3-phenylethylamine. Conditions glass column, 3 m X 3 mm I.D., 10% SE-30 on Chromo-sorb W (60-80 mesh, AW, silanized) nitrogen flow-rate, 35 ml/min temperature programme, 2°C/min (190-220°C), 3°C/min (220-250°C). (Reproduced from J. Chromatogr., 88 (1974) 373, by courtesy of S. Baba.)...

A solution of 100 p,g IgG in 500 (jlI 0.2 M NaHCO3/0.5 M NaCl (pH 8) was added to n-hydroxysuccinimidyl (NHS)-activated 6-aminohexanoic acid-coupled sepharose (Sigma, St Louis, USA), and allowed to bind for 60 min at 20 C before transferring onto a microcapillary (MoBiTec, Gottingen, Germany). Columns were washed alternately with blocking (ethanolamine/NaCl) and washing buffer (NaAc/NaCl). 

Remove the ethanolamine soludon by careful filtradon on the glass sinter. Wash the gel alternately with at least three cycles of the acetate/saline and borate/saline buffers to remove noncovalendy adsorbed protein. Pour the gel into a glass chromatography column and equilibrate with phosphate/saline buffer. 

A murine monoclonal antibody, LG-85, specific for MlANS-labeled peptides and proteins was produced by the Hybridoma Development group at ImmunoGen, Inc. The antibody, an IgG was produced from the hybridoma grown as an ascites tumor in mice, and was purified from the ascites fluid by affinity chromatography over a Protein A-Sepharose colunm. The purified antibody was then used to prepare an LG-85-Protein G-Sepharose affinity colunm as follows Antibody in PBS was added to resin at a concentration of 2 mg LG-85/mL resin packed in a column. After incubation for 90 min, the resin was washed with 0.2 M borate buffer, pH 9.0, and dimethylpimylimidate was added to a concentration of 20 mM. After cross-linking for 30 min at ambient temperature, the reaction was quenched by incubation for 30 min with 2 M ethanolamine.HCl, pH 7.8. The column was subsequently equilibrated in PBS. 

Column Micropak SilO (250x2.1 mm ID), mobile phase hexanes - ethanol - ethanolamine (91.5 8.47 0.03), flow rate 1 ml/min, detection UV 235 nm. Peaks 1, quinidine 2, dihydroquinidine 3, 2 -quinidinone 4, primaquine 5, quinidine-N-oxide 6, 3-hydroxyquinidine. 

Chromatogram a, b and e column Radial-Pak C18 (100x8 mm ID), mobile phase acetonitrile - water - ethanolamine (45 55 0.1), flow rate 3 ml/min, detection UV 200 nm. 

Fig. 5-27. Separation of ethanolamines. — Separator column IonPac NS1 (10pm) eluent 0.004 mol/L hexanesulfonic acid + 0.04 mol/L H3B03 flow rate 1 mL/min detection suppressed conductivity injection volume 100 pL solute concentrations ammonium (1), 2.5 ppm monoethanol-amine (2), 5 ppm diethanolamine (3), and 10 ppm triethanolamine (4).

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