• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.154-160
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• 2017

BACKGROUND:This study was carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiency was compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODS AND RESULTS:The BPs (bisphenol A, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range of MDLs by SPE and LLE methods was $0.0005{\sim}0.0234{\mu}g/L$ and $0.0037{\sim}0.2034{\mu}g/L$, and that of LOQs was $0.0015{\sim}0.0744{\mu}g/L$ and $0.0117{\sim}0.6477{\mu}g/L$, respectively. The calibration curve obtained from standard solution of $0.004{\sim}4.0{\mu}g/L$ (SPE) and $0.016{\sim}16{\mu}g/L$ (LLE) showed good linearity with $r^2$ value of 0.9969 over. Accuracy was 93.2~108% and 97.4~120%, and precision was 1.7~4.6% and 0.7~6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPA were highest among the BPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in the Yeongsan river basin. The concentration of BPB, BPC, BPE, BPF and BPS were not detected in all sites, whereas BPA was ranged $0.0095{\sim}0.2583{\mu}g/L$, which was $0.0166{\sim}0.0810{\mu}g/L$ for mainstreams, $0.0095{\sim}0.2583{\mu}g/L$ for tributaries, $0.0352{\sim}0.1217{\mu}g/L$ for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS. We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.

• Journal of Korean Society of Environmental Engineers
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• v.29 no.6
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• pp.689-698
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• 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 $0.675\sim1.970{\mu}g/kg$.

• Analytical Science and Technology
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• v.14 no.6
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• pp.499-503
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• 2001

A new simple, rapid and sensitive gas chromatographic technique for the determination of bisphenol-A in can materials, which is the major material of epoxy resin and polycarbonate polymer, is proposed. This method is characterised by derivatization of the bisphenol-A with a acylating reagent forming the acetate derivative to optimize the chromatographic property. The detection of bisphenol-A is performed based on GC/MS (gas chromatography/mass spectrometry). Several beverages were analyzed by the proposed method for the determination of bisphenol-A Bisphenol-A was assayed the range of $0.11{\sim}11.40{\mu}g/can$ from the can materials.

• Analytical Science and Technology
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• v.21 no.1
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• pp.53-57
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• 2008

In order to survey the contents of ethyl carbamate in alcoholic beverages, GC/MS-SIM method was used after extraction with dichloromethane in solid phase extract cartridge contained alcoholic beverages. In the applied GC/MS-SIM method, the values of recoveries and relative standard deviation were ranged from 85.2 % to 87.9 % and from 0.7 % to 1.9 %, the limit of detection and quantification were $2{\mu}g/kg$ and $10{\mu}g/kg$. Depending on alcoholic beverage kinds, the levels were variable and the average level was $194{\mu}g/kg$ for liquor, $105{\mu}g/kg$ for fruit wine, $62{\mu}g/kg$ distilled spirit, $28{\mu}g/kg$ for sake, $15{\mu}g/kg$ for yakju, $12{\mu}g/kg$ for other alcohol beverages, ND for soju, respectively.

• Proceedings of the Korea Society of Environmental Toocicology Conference
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• 2003.05a
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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.

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

• Analytical Science and Technology
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• v.15 no.5
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• pp.475-481
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• 2002

The determination of phthalates and adipate in natural mineral water and its container is described. Phthalates and adipate were extracted from natural mineral water by liquid-liquid extraction with methylene chloride, concentrated and then injected in GC-MS (SIM). Phthalates and adipate from 1) PET, cap, label and glue were extracted in Soxhlet with 50 mL of carbon tetrachloride, purified with silicagel and detected with GC-MS (SIM). Peak shapes and quantitation of phthalates and adipate were excellent, with linear calibration curves over a range of $0.1{\sim}10{\mu}g/L$ in water sample ($r^2$ > 0.996) and over a range of $1{\sim}1,000{\mu}g/Kg$ in solid samples ($r^2$>0.994). The detection limits of analytes were $0.002{\sim}0.010{\mu}g/L$ in water and $0.01{\sim}0.02{\mu}g/Kg$ in solid samples. Five kinds of natural mineral water samples, two PETs, two labels, two caps and two glues were quantified by the described procedure. As a results, the concentrations of total phthalates in natural mineral water ranged from ND ~ 1.2 ng/mL. Otherwise, the concentrations of total phthalate extracted from PET ranged from 0.55 ~ 1.2 mg/Kg. We found that the accurate determination of phthalte and adipate in natural mineral water and container must be considered blank correction and the removal of label and glue in PET sample.

• Applied Biological Chemistry
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• v.47 no.1
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• pp.124-129
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• 2004

The composition of essential oils isolated from the aerial parts of Artemisia iwayomogi Kitamura and Artemisia capillaris Thunberg collected from two diffenent cultivation area, respectively, was analyzed by GC and GC-MS. Sixty components were identified in oils from A. iwayomogi. The major components of A. iwayomogi oil collected from one area (Sample A) were iso-pinocamphone (31.64%), 1,8-cineo1e (21.55%), ${\beta}-pinene$ (4.46%), pinocarvone (3.72%), myrtenal (3.42%) and trans-pinocarve1 (3.14%), and the major components of the oil from the other area (Sample B) were camphor (26.99%), 1,8-cineo1e (21.55%), ${\alpha}-terpineol$ (7.63%), borneol (4.10%), camphene (3.97%) and artemisia ketone (3.84%). Eighty components were identified in oils from A. capillaris. The major components were capillene $(26.01{\sim}30.31%)$, ${\beta}-pinene(8.55{\sim}18.38%)$, ${\beta}-caryophyllene(8.80{\sim}13.70%)$, ${\beta}-himachalene(1.67{\sim}5.57%)$, $cis,trans- {\alpha}-farnesene(2.10{\sim}7.38%)$ and germacrene D $(2.27{\sim}5.46%)$ and there was no difference in oil composition of A. capillaris between two cultivation area.

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

• Analytical Science and Technology
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• v.18 no.4
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• pp.320-328
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• 2005

The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).