Separation and concentration of biologically active compounds by capillary electrophoresis using modifiers based on imidazolium cation

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Аннотация

A cationic covalent coating of quartz capillary walls based on imidazolium cation was synthesised; the reproducibility by electroosmotic flow (marker dimethylformamide) was 99 %. The conditions (concentration and pH of background electrolyte, nature and volume of organic additive) for their separation by capillary electrophoresis were optimised on model systems of phenyl- and indolecarboxylic acids (phenyl lactic, phenylanthanoic, phenyl butanoic, indole lactic, indolpropionic, indolacrylic hydroxymindal, homogentisic, homovanilinic, hydroxindoleacetic acids): 10 mM phosphate buffer solution with pH 4.2 with addition of 10 vol. % acetonitrile. The resolution factors of neighbouring pairs of analytes ranged from 1.7 to 18.9. The possibility of intracapillary concentration of phenyl- and indolecarboxylic acids using the synthesised coating was shown. Electrostacking allowed to concentrate the analytes 106–512 times and to lower the detection limits to 4–72 ng/ml.

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Авторлар туралы

A. Ganieva

St. Petersburg State University

Хат алмасуға жауапты Автор.
Email: st110520@student.spbu.ru
Ресей, Saint-Petersburg

L. Kartsova

St. Petersburg State University

Email: st110520@student.spbu.ru
Ресей, Saint-Petersburg

Әдебиет тізімі

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Әрекет
1. JATS XML
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2. Fig. 1. Scheme of synthesis of covalent coating without the stage of postfunctionalization of imidazole.

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3. Fig. 2. Scanning electron micrograph of unmodified capillary (left) and imidazole-modified capillary (right).

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4. Fig. 3. (a) Schematic diagram of the covalent coating based on the imidazolium cation, (b) values ​​of the resolution factors for separating a model mixture of phenyl- and indolecarboxylic acids at different pH values ​​of the background electrolyte, (c)–(e) electropherograms of model mixtures of phenyl- and indolecarboxylic acids on a covalent coating based on the imidazolium cation.

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5. Fig. 4. Electropherogram of a model mixture of phenyl- and indolecarboxylic acids (c = 5–100 μg/ml) (a) on an unmodified capillary, (b) on a dynamic coating based on CTAB, (c) on a butylimidazolium coating, (d) on an octylimidazolium coating. Conditions: capillary electrophoresis system KAPEL®-105M; 5 s × 30 mbar; background electrolyte: 10 mM phosphate buffer solution with pH 4.2 + 10 vol. % acetonitrile; –20 kV; 220 nm.

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6. Fig. 5. Electropherograms of a model mixture of phenyl and indole carboxylic acids on a covalent coating based on the imidazolium cation: (a) stacking with a large volume of introduced sample, (b) stacking with field enhancement and a water plug (b), electrostacking (c), (d) stacking with field enhancement and a micellar plug.

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7. Fig. 6. Electropherogram of separation of a model mixture of biogenic amines on an imidazolium coating. Conditions: capillary electrophoresis system KAPEL®-105M, 2 s × 30 mbar; background electrolyte: 10 mM phosphate buffer solution with pH 2; –20 kV; 220 nm. Analytes: MN – metanephrine, AD – adrenaline, NA – noradrenaline, NMN – normetanephrine, 5-HT – serotonin, DHBA – 3,4-dihydroxybenzylamine.

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