• Title/Summary/Keyword: GC-MS-SIM

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Combined Isobutoxycarbonylation and tert-Butyldimethylsilylation for the GC/MS-SIM Detection of Alkylphenols, Chlorophenols and Bisphenol A in Mackerel Samples

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.26 no.9
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    • pp.697-705
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    • 2003
  • The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

Study on measurement of DNA adducts formed in liver cells and bladder epithelial cells of rats exposed dichlorobenzidine(DCB) by $^{32}$ P-postlabeling and GC/MS-SIM method (디클로로벤지딘에 폭로된 흰쥐의 간장세포와 방광 상피세포에 형성된 DNA adducts의 $^{32}$ P-postlabeling과 GC/MS-SIM에 의한 분석)

  • Lee Jin Heon;Shin Ho-Sang;Jang Mi Seon
    • Journal of Environmental Health Sciences
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    • v.28 no.1
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    • pp.21-29
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    • 2002
  • To identify and evaluate the dichlorobenzidine(DCB)-DNA adducts in liver cell and bladder epithelial cells by $^{32}$ P-postlabeling and GC/MS-SIM, we orally exposed the dichlorobenzidine(20mg/kh body wt./day) to male Sprague-Dawley rats(l85$\pm$10g) for 14 days. Two kinds of DCB-DNA adduct(A1 and A2) were found at the same site of thin layer chromatogram of $^{32}$ P-postlabeling method in liver cells and bladder epithelial cells. In liver cells, relative adduct labeling(RAL) $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 34.1$\pm$3.71 and 69.9$\pm$5.02, that of adduct A2 were 74.1$\pm$10.1 and 105.1$\pm$10.1 on 10 and 14 days after treatment, respectively. And in bladder epithelia cells, RAL $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 5.92$\pm$1.60 and 15.9$\pm$1.31, that of adduct A2 were 9.81$\pm$2.81 and 22.8$\pm$1.79 on 10 and 14 days after treatment, respectively. DCB metabolites formed DNA adducts were monoacetyl-dichlorobenzidine(acDCB) and diacetyl-dichlorobenzidine(di-acDCB), which was identify by gas chromatography/mass spectrometry-scan ionization mode(GC/MS-SIM), after hydrolysis of DCB-DNA adducts isolated from live cells and bladder epithelial cells. The base peak of acDCB were 252 and 294 m/z, and that of di-acDCB were 252, 294 and 336 m/z. In conclusion, the exposed DCB formed two kinds of DCB-DNA adduct, the proximate materials of that were acDCB and di-acDCB in liver and bladder epithelial cells. And the above GC/MS-SIM method was found the DCB-DNA adducts could be monitoring by gas chromatography.

Sensitive Determination of Alkylphenols, Chlorophenols, and Bisphenol A using GC/MS-SIM in Papers Materials

  • Kim, Hyub;Kim, Jin-Ho;Kim, Yong-Hwa
    • Proceedings of the PSK Conference
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    • pp.120.2-121
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    • 2003
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. (omitted)

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Dertermination of Alkylphenols, Chlorophenols and Bisphenol A in Various Samples by Freezing Filtration and GC/MS-SIM

  • Kim, Hyub
    • Proceedings of the PSK Conference
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    • pp.68.1-68
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    • 2003
  • A method for determination 11 endocrine disrupting chemicals of phenols in various samples was deloped. The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization method and tert-butyldimethylsilyl (TBDMS) derivatization method. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at -60$^{\circ}C$ for 2 hours (freezing filtration). (omitted)

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Quantitative Analysis of Pentachlorophenol in Paper Products (종이재 중의 Pentachlorophenol 정량 분석)

  • Hahn, Airan;Park, Jihye;Choi, Hyeongki;Hong, Sungyeap;Han, Hyechul;Jo, Byoungmuk;Oh, Jungsoo
    • Applied Chemistry for Engineering
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    • v.16 no.3
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    • pp.323-327
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    • 2005
  • Pentachlorophenol (PCP) is a representative compound of chlorophenol derivatives which are especially toxic and potentially carcinogenic compounds in the priority pollutant list of the EPA (Environmental Protection Agency, USA). The aim of this study was to investigate an analysis method of PCP in infinitesimal quantity retained in paper. PCP in paper was pretreated by solid phase extraction (SPE) in a phenyl cartridge. The extracted sample was acetylated or silylated and analyzed with GC/MS-SIM. The detection sensitivity of silylated PCP was improved significantly when compared with those of PCP itself and acetylated PCP. As a test specimen, an office paper and a wallpaper were used.

Analysis of Octylphenol, Nonylphenol, Di-octylphthalate in Sewage Sludge by GC/MS-SIM (GC/MS-SIM에 의한 하수 슬러지중에 포함된 Octylphenol, Nonylphenol, Di-octylphthalate의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.248-255
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    • 1999
  • Sewage sludge samples were extracted with dichlomethane by Soxhlet extraction. The extracts were analysed for the endocrine disrupting compounds (EDC), octylphenol(OP), nonylphenol (NP) and bis (2-ethylhexyl)phthalate (DOP) using GC/MS-SIM. In industrial sewage sludge (sample Z-1) the concentration of NP and DOP were respectively $1168{\mu}g/g$ and $1172{\mu}g/g$ whereas in domestic sludge (sample Z-2) the concentration were respectively $10.8{\mu}g/g$ and $80{\mu}g/g$. OP was not detected in Z-2, but detected a small amount in Z-2 of the samples. Environmental EDC have been shown to affect the fertility of range of living organisms, including humans, and the high levels of NP and DOP in industrial sewage sludge could have serious implications for the reproductive health of humans particularly if the compounds entered the human food chain through water or the ingestion of vegetables or animal products.

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디클로벤지딘에 폭로된 흰쥐의 간장세포와 방광 상피세포에 형성된 DNA adducts의 $^{32}P-postlabeling$과 GC/MS-SIM에 의한 분석

  • 이진헌;신호상;장미선
    • Proceedings of the Korean Environmental Health Society Conference
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    • pp.49-51
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    • 2002
  • To identify and evaluate the dichlorobenzidine(DCB)-DNA adducts in liver cell and bladder epithelial cells by $^{32}$ P-postlabeling and GC/MS-SIM, we orally exposed the dichlorobenzidine (20mg/kh body wt.,/day)to male sprague-dawley rats for 14 days. Two kinds of DCB-DNA adduct were found at the same site of thin layer chromatogram of $^{32}$ P-postlabeling method in liver cells and bladder epithelial cells. In liver cells, relative adduct labeling(RAL) $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 34.1$\pm$3.71 and 69.9$\pm$5.02, that of adduct A2 were 74.1$\pm$10.1 and 105.1$\pm$10.1 on 10 and 14 days after treatment, respectively. And in bladder epithelia cells, RAL $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 5.92$\pm$1.60 and 15.9$\pm$1.31, that of adduct A2 were 9,81$\pm$2.81 and 22.8$\pm$1.79 on 10 and 14 days after treatment, respectively. DCB metabolites formed DNA adducts were monoacetyl-dichlorobenzidine(acDCB) and diacety1-dichlorobenzidine(di-acDCB), which was identify by gas chromatography/mass spectrometry-scan ionization mode(GC/MS-SIM), along with hydrolysis, extraction and TFA(trifluoroacetyl anhyride) derivatization with DCB-DNA adducts isolated from live cells and bladder epithelial cells. The base peak of acDCB were 252 and 294 m/z, and that of di-acDCB were 252, 294 and 336 m/z. In conclusion, the exposed DCB formed two kinds of DCB-DNA adduct, the proximate materials of that were acDCB and di-acDCB in liver and bladder epithlial cells. And the above GC/MS-SIM method was found the DCB-DNA adducts could be monitoring by gas chromatography.

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GC/MS-SIM for the Determination of Alkylphenols, Chlorophenols and Bisphenol A in Paper Materials

  • Kim, Hyub
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • pp.145-145
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    • 2003
  • A method for the determination of alkylphenols, chlorophenols and bisphenol A in paper materials using GC/MS-SIM has been developed. Eleven endocrine disrupting chemicals (EDCs) of phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 82.4∼108.8 % by area ratio of pheranthrene-d$\sub$10/ vs bisphenol A d$\sub$l6/. (isoBOC derivatization and TBDMS derivatization) The SIM responses were linear with the correlation coefficient varying 0.9717∼0.9995 (isoBOC derivatization), and 0.9842∼0.9980 (TBDMS derivatization). The range of concentrations was respectively, 0.95∼l.44 ng/g in 2,4-dichlorophenol, 1.01∼1.17 ng/g in t-butylphenol, 2.17∼5.84 ng/g in pentachlorophenol, 12.68∼14.88 ng/g in nonylphenol and 30.84∼153.72 ng/g in bisphenol A.

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