Chromatographic Determination of Carbonyl Compounds as Their 2,4-Dinitrophenylhydrazones I. Gas Chromatography

Simultaneous determination of formic acid and formaldehyde in pharmaceutical excipients using headspace GC/MS

“…These challenges can generally be overcome by the derivatization and subsequent determination of their derivatives using GC or high performance liquid chromatography (HPLC) techniques. Various derivatization methods followed by GC or HPLC determination of formic acid or formaldehyde have been reported [14][15][16][17][18][19][20][21][22] but the sample preparation generally involves complex chemical reactions and the methods are not suitable for the simultaneous determination of formic acid and formaldehyde in excipient matrices. A critical step in the method development was to find a suitable derivatization reagent.…”

Synthesis of short-chain hydroxyaldehydes and their 2,4-dinitrophenylhydrazone derivatives, and separation of their isomers by high-performance liquid chromatography

“…The product was obtained in form of yellow crystals (220 mg, 0.82 mmol, 22%). 1 4,4-Dimethoxybutan-2-one (985 mg, 7.46 mmol) was dissolved in MeCN (200 mL) and H 2 SO 4 (1.00 g, 10.20 mmol) and water (38.9 mmol) were added and stirred at rt for 2.5 h. The pH was adjusted to 5.0 by addition of KHCO 3 , then Na 2 SO 4 (5 g) and (2,4-dinitrophenyl)hydrazine (stabilized with 50 wt% water, 2.95 g, 7.46 mmol) were added and the mixture was stirred for 1 h, then neutralized with KHCO 3 (pH = 7.0), filtered and evaporated. An analytically pure sample (30 mg, 0.11 mmol) was obtained by semipreparative HPLC (Acetonitrile).…”

“…These are stable, non-volatile and often crystalline solids with a sharp melting point. Aldehydes and their DNPH derivatives can be determined by gas chromatography [1,2] or by HPLC on standard C 18 -phases, commonly using water (or buffer)/acetonitrile (MeCN) mixtures as eluent (in some cases with additional methanol, isopropanol and/or tetrahydofurane) [3][4][5][6][7]. Unfortunately, these methods do not allow separation of structural isomers such as butyraldehyde DNPH and isobutyraldehyde DNPH or their hydroxy analogues [3][4][5][6][7].…”

Chemosorption sampling and analysis of formaldehyde in air. Influence on recovery during the simultaneous sampling of formaldehyde, phenol, furfural and furfuryl alcohol.

“…In order to obtain higher sensitivity, the formation of hydrazones, which can be used both for GC and HPLC analysis, has been utilized. The most frequently used are the 2,4-dinitrophenylhydrazones (1,4,5,7,9,12,13,16,19,20,23,24,26,28,29,30), but pentafluorophenylhydrazones (8,15) and, for HPLC, the dansylhydrazones (6,12) have also been demonstrated to be useful.…”