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A simple synthetic route for the preparation of a reversed-phase stationary phase based on monosized-porous hydrogel beads and its chromatographic use for separation of small molecules

Çelebi B.

Acta Chromatographica

2017

Vol. 29, no. 2

143--159

New polyacrylate-based monosized-porous polymer beads were proposed as a stationary phase for the separation of polar compounds by microbore reversed-phase chromatography. For this purpose, monosized-porous poly(glycerol dimethacrylate-co-glycerol-1,3-diglycerolate diacrylate), poly(GDMA-co-GDGDA), beads with hydroxyl functionality were synthesized by a modified seeded polymerization. The selected octadecylating agent, stearoyl chloride (SC), was covalently attached onto the hydrophilic beads via a direct, single stage reaction with a simple synthetic route. SC attached-poly( GDMA-co-GDGDA) beads were slurry-packed into the microbore columns and used as separation medium microbore reversed-phase chromatography. The stationary phase was used for separation of alkylbenzenes and polar analytes by micro reversed-phase chromatography, using mobile phases with low acetonitrile content. Theoretical plate number (TPN) values up to 12,000 plates m−1 and 10,000 plates m−1 for alkylbenzenes and polar analytes, respectively, were achieved. The results also showed that poly(GDMA-co-GDGDA) hydrogel beads are a promising starting material for a number of chromatographic applications like reversed-phase (RP) chromatography, hydrophilic interaction chromatography (HILIC), ion-exchange chromatography (IEC), and affinity chromatography with a single-stage surface modification.

Estryfikacja alifatycznych oligoeteroalkoholi chlorkiem kwasu stearynowego

Nowicki J., Wasilewski J., Góralczyk K., Lukosek M.

Przemysł Chemiczny

2004

T. 83, nr 3

130-132

Przedstawiono wyniki badań estryfikacji wybranych oligoeteroalkoholi (Bikanoli) przy użyciu chlorku kwasu stearynowego. Stwierdzono, że synteza przebiega w temp. 85-88°C z wydajnością estrów 90-91 % mas. dla optymalnego stosunku molowego alkohohchlorek wynoszącym 1,05:1

2-(2-Methoxyethoxy)-, 2-[2-(2-methoxyethoxy)ethoxy]-, 2butoxy-, or 2-(2-butoxyethoxy)-ethanol was esterified hot with stearoyl chloride, the evolving HCI was removed with a water injector, the mixt. after the reaction was stirred 1 h at 80°C, and the resulting ester (yield 90-91%, selectivity 95+ %, acid no. 6.4-6.6 mg KOH/g) was washed with water until neutral and dehydrated at 110°C in N2. Box-Benken's design experiments showed reaction temp. and reactant mole rafio to be optimum at 85-88°C and 1.05-1.07, resp.