ХРОМАТОМАСС-СПЕКТРОМЕТРИЧЕСКАЯ ХАРАКТЕРИСТИКА ДИЭТИЛКЕТАЛЕЙ АЛИФАТИЧЕСКИХ КАРБОНИЛЬНЫХ СОЕДИНЕНИЙ
Аннотация
Несколько (10) гомологов диэтилкеталей алифатических карбонильных соединений синтезированы из соответствующих карбонильных соединений и ортоэтилформиата в присутствии каталитических количеств серной кислоты или гидросульфата магния на силикагеле. Все продукты охарактеризованы масс-спектрами с ионизацией электронами и газохроматографическими индексами удерживания на стандартных неполярных полидиметилсилоксановых неподвижных фазах. Из характеристик гомологических рядов определены разности индексов продуктов и исходных субстратов, составляющие для диэтилкеталей и этил-(1-алкениловых) эфиров 266 ± 26 и 99 ± 20 ед. индекса, соответственно. Такие параметры позволяют предсказывать положение пиков ранее не охарактеризованных соединений этих рядов по индексам удерживания исходных карбонильных соединений. Другой характеристикой гомологов, объединяющей их масс-спектрометрические и хроматографические параметры, являются гомологические инкременты индексов удерживания: iRI = RI – 100x, где х = int(M/14), int – функция, обозначающая целую часть частного от деления молекулярного массового числа на 14, эквивалентная записи M = 14x + y, у – номер гомологической группы соединения, yM º M(mod14). Такие инкременты позволяют по хроматографическим данным оценивать молекулярные массы аналитов, не дающих в масс-спектрах надежно регистрируемых сигналов молекулярных ионов, а также контролировать результаты идентификации с целью предотвращения ошибок.
Ключевые слова: Диэтилкетали алифатических кетонов, этил-(1-алкениловые) эфиры, газовая хроматография, масс-спектрометрия, разности индексов удерживания диэтилкеталей и соответствующих кетонов, гомологические инкременты индексов удерживания.
DOI: http://dx.doi.org/10.15826/analitika.2019.23.3.009Полный текст:
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