Chinese Journal of Chromatography

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Application of single drop microextraction in the determination of phthalate esters and parabens in drugs by gas
chromatography-mass spectrometry

QI Aiming, LI Meigui, MAO Liqiu   

  1. Hunan Normal University, Key Laboratory of Chemical Biology and Traditional Chinese Medicine
    Research, Ministry of Education, Changsha 410081, China
  • Received:2007-09-14 Revised:2007-11-09 Online:2008-05-30 Published:1984-03-25
  • Contact: MAO Liqiu

Abstract:

Single drop microextraction (SDME) was used for the determination of phthalate esters and parabens in drugs by gas chromatography-ion trap mass spectrometry (GC-IT/MS). The effects of the nature of extraction solvents, microdrop volume, the depth of microdrop in sample solution, extraction time and stirring rate on the extraction efficiency were investigated separately. The optimal SDME conditions, 1.5 μL of toluene, 0.8 cm of the depth of microdrop, 1000 r/min of stirring rate and 20 min of extraction time, were obtained and used for the analysis of methylparaben (MP), ethylparaben (EP), propylparaben (PP), iso-propylparaben (IPP), butylparaben (BP), dimethyl phthalate (DMP), diethyl phthalate (DEP) and dibutyl phthalate (DBP) in drugs. The results showed that the working curves for 8 phthalate esters and parabens were linear in the range of 0.032-80 mg/L by GC-MS on selective ion storage mode. The limits of detection (LOD) were between 0.6 μg/L and 1.28 mg/L, the overall recoveries were 95.85%-148.85% with the relative standard deviations of 3.9%-14.9%.

Key words: drug
,
gas chromatography-ion trap mass spectrometry (GC-IT/MS), parabens, phthalate esters, single drop microextraction (SDME)