Salt-assisted liquid-liquid microextraction with water-miscible organic solvents for the determination of carbonyl compounds by high-performance liquid chromatography.
A simple and rapid method has been reported for the determination of carbonyl compounds involving reaction with 2,4-dinitrophenylhydrazine and extraction of hydrazones with water-miscible organic solvent acetonitrile when the phase separation occurs by addition of ammonium sulphate, a process called salt-assisted liquid-liquid microextraction. The extract was analyzed by high-performance liquid chromatography with UV detection at 360 nm. The procedure has been optimized with respect to solvent suitable for extraction, salt for phase separation between water and organic solvent, reaction temperature and reaction time. The method has been validated when a linear dynamic range was obtained between the amount of analyte and peak area of hydrazones in the range 7 microg-15 mg L(-1), the correlation coefficient over 0.9964-0.9991, and the limit of detection in the range 0.58-3.2 microg L(-1). Spiked water samples have been analyzed with adequate accuracy, and application of the method has been demonstrated in the analysis of benzaldehyde formed as oxidation product in pharmaceutical preparation where benzyl alcohol is used as preservative, and for a keto drug dexketoprofen.
Gupta
Manju
M
Department of Chemistry, Rani Durgavati University, Pachpedi, Jabalpur, Madhya Pradesh, India.
Jain
Archana
A
Verma
Krishna K
KK
D000447:Aldehydes / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D001547:Benzaldehydes / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D005591:Chemical Fractionation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003512:Cyclohexanones / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D005618:Fresh Water / Q000032:analysis / Q000737:chemistry; D007659:Ketones / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D007660:Ketoprofen / Q000031:analogs & derivatives / Q000032:analysis / Q000737:chemistry; D015394:Molecular Structure; D009930:Organic Chemicals / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000032:analysis / Q000737:chemistry; D010659:Phenylhydrazines / Q000737:chemistry; D015203:Reproducibility of Results; D012997:Solvents / Q000737:chemistry*; D014325:Tromethamine / Q000031:analogs & derivatives / Q000032:analysis / Q000737:chemistry; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000737:chemistry
D000447:Aldehydes; D001547:Benzaldehydes; D003512:Cyclohexanones; D007659:Ketones; D009930:Organic Chemicals; D004364:Pharmaceutical Preparations; D010659:Phenylhydrazines; D012997:Solvents; D014874:Water Pollutants, Chemical; D014325:Tromethamine; D014867:Water; C004787:2,4-dinitrophenylhydrazine; C036468:cyclohexanone; D007660:Ketoprofen; C118296:dexketoprofen trometamol; C032175:benzaldehyde