• Analytical Science and Technology
• /
• v.15 no.3
• /
• pp.196-213
• /
• 2002

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison; EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. 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 85.1~109.9% (EPA method) and 90.3~126.6% (isoBOC derivatization and TBDMS derivatization), respectively. The method detection limit of bisphenol A for SIM were 0.732 ${\mu}g/{\ell}$ (EPA method), 0.002 ${\mu}g/{\ell}$ (isoBOC derivatization) and 0.021 ${\mu}g/{\ell}$ (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981 (isoBOC derivatization), and 0.9908~0.9996 (TBDMS derivatization). When these methods were applied to treated wastewater sample from a polyethylene plant, the concentrations of 11 phenols were below the method detection limit.

• Proceedings of the Korea Society of Environmental Toocicology Conference
• /
• 2003.10a
• /
• pp.149-149
• /
• 2003

A new technique is proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert.-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6∼105.2 % (isoBOC derivatization) and 97.6∼484.5 % (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001∼0.050 $\mu\textrm{g}$/l (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/l (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). The derivative methods and their application to tap water samples will be disscussed.

• Environmental Engineering Research
• /
• v.13 no.4
• /
• pp.216-223
• /
• 2008

An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

• Environmental Analysis Health and Toxicology
• /
• v.18 no.3
• /
• pp.199-208
• /
• 2003

A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the CC/MS SIM mode. The recoveries were 86.6 ∼ 105.2％ (isoBOC derivatization) and 97.6∼484.5％ (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol h for SIM were 0.001∼0.050 $\mu\textrm{g}$/1 (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/1 (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). When these methods were applied to tap water samples, the range of concentrations were 22.8∼31.3 ng/1 in 2,4-dichlorophenol, 28.6∼70.3 ng/1 in pentachlorophenol, 15.2∼17.4 ng/1 in t-butylphenol, 10.8∼13.2 ng/1 in t-octylphenol and 17.6∼36.3 ng/l in bisphenol A, respectively.

• Environmental Analysis Health and Toxicology
• /
• v.18 no.1
• /
• pp.45-55
• /
• 2003

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-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. 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 SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8％) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 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.

• Archives of Pharmacal Research
• /
• v.26 no.9
• /
• pp.697-705
• /
• 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.

• Proceedings of the Korea Society of Environmental Toocicology Conference
• /
• 2003.05a
• /
• pp.145-145
• /
• 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.

• Environmental Analysis Health and Toxicology
• /
• v.17 no.1
• /
• pp.37-51
• /
• 2002

Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9％ and 90.3∼126.6％ for the US-EPA method and the isoBOC.

• Proceedings of the PSK Conference
• /
• 2002.10a
• /
• pp.235.2-236
• /
• 2002

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison: EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. (omitted)

• Journal of Korean Society of Environmental Engineers
• /
• v.29 no.6
• /
• pp.689-698
• /
• 2007

A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.