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헤드스페이스-가스크로마토그래피-질량분석법에 의한 체모 중 포름알데하이드 측정법 연구
신호상,안혜실,Shin Ho-Sang,Ahn Hye-Sil 한국환경보건학회 2006 한국환경보건학회지 Vol.32 No.1
A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.
에틸렌옥사이드에 폭로된 흰쥐의 혈액에 형성된 헤모글로빈 부가체에 대한 연구
이진헌,신호상,안혜실,Lee Jin-Heon,Shin Ho-Sang,Ahn Hye-Sil 한국환경보건학회 2006 한국환경보건학회지 Vol.32 No.2
Ethylene oxide is a genotoxic carcinogen with widespread uses as industrial chemical intermediate and gaseous sterilant. 2-hydroxyethylated N-terminal valine in Hb is a good biomarker for biological monitoring of ethylene oxide exposure, because of its stability. For measuring the hemoglobin adduct formed by exposure of ethylene oxide, we studied the determination of (N-2-hydroxy-ethyl)valine(HEV) in hemoglobin adduct by using GC/MS. Firstly we synthesized HEV with 2-amino-ethanol and bromoisovaleric acid(BIVA) and confirmed it with GC/MS-FID. Its fragmentations were m/z 116(base ion, M+-45) and m/z 130(M+-31). For measuring HEV with higher sensitivity, we use derivatives which were PFPITH(pentafluorophenylisothiocianate) and TBDMS (tributyldimethylsilylation) by using Edman procedure. Its fragmentation were m/z 425(M+-57), m/z 383(M+-99) and m/z 172(M+-310) by using GC/MS. We did biological monitoring for mice inhalation exposure with 400 ppm ethylene oxide. The concentrations of hemoglobin adduct were $168{\pm}3.8\;and\;512{\pm}04$(nmol g-1 globin) at 0.5 hr/day 400 ppm ethylene oxide inhalation exposure group, and $631{\pm}17\;and\;2265{\pm}9.4$(nmol g-1 globin) at 1.0 hr/day 400 ppm ethylene oxide inhalation exposure for 1 and 4 weeks, respectively. We confirmed that (N-2-hydroxy-ethyl)valine(HEV) of hemoglobin was a good biomarker for biomonitoring of ethylene oxide exposure, and can measured with derivatives such as PFPITH(pentafluorophenylisothiocianate) and TBDMS(tributyldimethylsilylation) by using GC/MS.