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Unequivocal structural assignment of steroids in galenic emulsions employing HPLC‐nMR coupling
Author(s) -
Glaser Tobias,
Albert Klaus
Publication year - 2002
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/1615-9314(20020501)25:7<393::aid-jssc393>3.0.co;2-s
Subject(s) - chemistry , chromatography , elution , high performance liquid chromatography , gradient elution , proton nmr , methanol , analytical chemistry (journal) , organic chemistry
The structural identity of two steroidal components in the low μg range of a pharmaceutical gel was determined by a rapid and efficient analytical method employing on‐line HPLC‐NMR coupling. The chromatographic separation conditions were optimised towards the requirements of on‐line 1 H NMR detection, employing a tailored C 30 column together with a gradient elution of a methanol/D 2 O mixture. Stopped‐flow 1D and 2D 1 H NMR spectra of the investigated chromatographic peaks unequivocally revealed the structure of the corresponding steroids norethisterone acetate and estradiol.