• Title/Summary/Keyword: GC-MS-SIM

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Assessment of the Human Risk by an Intake of Ethyl Carbamate Present in Major Korean Fermented Foods

  • Noh, I-Woo;Ha, Mi-Sun;Han, Eun-Mee;Jang, In-Sook;An, Youn-Joo;Ha, Sang-Do;Park, Sang-Kyu;Bae, Dong-Ho
    • Journal of Microbiology and Biotechnology
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    • v.16 no.12
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    • pp.1961-1967
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    • 2006
  • Levels of ethyl carbamate, a potential carcinogen produced naturally during fermentation, in major Korean fermented foods and alcoholic beverages were determined by GC/MS/SIM, and their average daily intake and excess cancer risk in Korean people were estimated. In GC/MS/SIM analysis n.d.-4.26, 1.40-58.90, n.d.-3.76, n.d.-1.87, and 0.40-10.07 $\mu$g/kg of ethyl carbamate were detected in kimchi, soy sauces, fermented pastes, fermented dairy products, and alcoholic beverages, respectively. The average daily intake of ethyl carbamate and excess cancer risk through major Korean fermented foods and alcoholic beverage consumption were 6.0 ng/kg bw/day and $3.0\times10^{-7}$, respectively for the average Korean person aged 3-64 years, and were mainly contributed by Chinese cabbage kimchi, soy sauces, and Soju.

Extracts and Essential Oil of Ledum palustre L. Leaves and Their Antioxidant and Antimicrobial Activities

  • Kim, Dong-Myong;Nam, Bong-Woo
    • Preventive Nutrition and Food Science
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    • v.11 no.2
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    • pp.100-104
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    • 2006
  • The in vitro antimicrobial and antioxidant activities of the essential oil and methanol extracts of Ledum palustre L. were investigated. Using GC-MS analysis, we identified 37 compounds in the essential oil, constituting 87.58% of the total oil. There are several monoterpenes, of which sabinene is the major compound ($16{\sim}17%$). There are several oxygenated monoterpenes of which terpinen-4-ol(7.6%) and myrtenal (3.5%) are the main constituents. $\beta$-Selinene, a-selinene, $\gamma$-elemene, a-caryophyllene are the main sesquiterpenes ($2{\sim}6%$ range). The oil strongly reduced the diphenylpicrylhydrazyl radical ($IC_{50}=1.56{\mu}g/mL$) formation and exhibited a hydroxyl radical scavenging effect in the $Fe^{3+}-EDTA-H_2O_2$ deoxyribose system ($IC_{50}=2.7{\mu}g/mL$), and also inhibited the nonenzymatic lipid peroxidation of rat liver homogenate ($IC_{50}=13.5{\mu}g/mL$). The polar phase of the extract showed antioxidant activity. The oil showed antimicrobial activity against Streptococcus pneumoniae, Clostridium perfringens, Candida albicans, Mycobacterium smegmatis, Acinetobacter lwoffii and Candida krusei while the water-insoluble parts of the methanolic extracts exhibited slight or no activity. This study confirms that the essential oil of Ledum palustre L. possesses antioxidant and low antimicrobial properties in vitro.

A Study on Nonylphenol, Octylphenol, and Di (2-ethylhexyl)phthalate in Sewage Sludge (하수슬러지 중 Nonylphenol, Octylphenol, Di (2-ethylhexyl)phthalate 의 연구)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.451-458
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    • 2002
  • Determination were performed for the presence of three common environmental endocrine disrupting compounds (EDC), namely nonylphenol (NP), octylphenol (OP), di (2-ethylhexyl)phthalate in sewage sludge from 67 wastes plants, using Soxhlet extraction and GC/MS-SIM. NP and DEHP were detected in almost every sludges but OP was not detected. The range and mean value for NP of all sludge samples were nd~593, $62{\mu}g/g$ dry and the two statistic values for DEHP of those were 13~4733, $1176{\mu}g/g$ dry respectively. DEHP content was 20 times greater than NP in sludges. Concentrations of NP and DEHP in sludge from individual area were increased as following order ; Jeolla South and North Province (Cheju) < Chungcheong South and North Province (Kwangwon) < Gyungsang South and North Province < Wide City < Kyunggi Province.

Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization (Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석)

  • Ahn, Yun Gyong;Lee, Jee Yeon;Kim, Jeehyeong;Hong, Jongki
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.458-465
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    • 2003
  • The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

Estimation of Korean Adult's Daily Intake of Ethyl Carbamate through Korean Commercial Alcoholic Beverages Based on the Monitoring

  • Ha, Mi-Sun;Hu, Soo-Jung;Park, Hee-Ra;Lee, Hyo-Min;Kwon, Ki-Sung;Han, Eun-Mee;Kim, Kyung-Mi;Ko, Eun-Jung;Ha, Sang-Do;Bae, Dong-Ho
    • Food Science and Biotechnology
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    • v.15 no.1
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    • pp.112-116
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    • 2006
  • Levels of ethyl carbamate, by-product produced naturally during fermentation, in Korean alcoholic beverages were determined by Gas Chromatography/mass spectrometry/selected ion mode (GC/MS/SIM), and their daily intake by Korean adult group was estimated. In GC/MS/SIM analysis 0.8-10.1, 0.5-0.8, 0.4-0.9, 3.5-689.9, 8.4-30.3, 13.9-30.0, and 1.7-11.7 ppb of ethyl carbamate were detected in soju, beer, takju, fruit wine, cheongju, whiskey, and grape wine, respectively. Maximum daily exposure of ethyl carbamate through alcoholic beverage consumption was 7.41 ng/kg body weight/day for average Korean male, with one soju brand and two fruit wine brands showing high ethyl carbamate level.

Monitoring of Pesticide Residues and Risk Assessment of Agricultural Products Consumed in South Korea (국내유통농산물 중 잔류농약 모니터링 및 안전성 평가)

  • Kim, Sung-Hun;Choe, Won-Jo;Baik, Yong-Kyoo;Kim, Woo-Seong
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.11
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    • pp.1515-1522
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    • 2008
  • Monitoring the pesticide residues in agricultural products is essential to protect consumers, obtain data for risk assessment, and ensure fair trade practices. We developed a multi-residue method for the analysis of 37 pesticides with different physico-chemical properties in agricultural products and analyzed the amount of pesticide residues on about 1,000 samples circulated in South Korea. The samples consisted of 26 different types of agricultural products selected at markets in 14 major cities; cereals (2 species), nuts (1 species) potatoes (1 species), beans (2 species), fruits (3 species), vegetables (16 species), and mushrooms (1 species). In this study, residual pesticides were detected in 23 samples (2.2%) and one sample was detected to be over maximum residue limits (MRLs, 0.1%) for pesticides in foods by the Korea food code. In leafy vegetables such as pepper leaves, radish leaves, cham-na-mul, shin-sun-cho, crown daisy, chwi-na-mul and citrus fruits such as kumquat, 8 kinds of pesticides were detected. Specially, diazinon were detected over MRLs and also, endosulfan, ethoprophos and phenthoate were detected frequently. Based on these results, we investigated the risk assesment from amount of residual pesticide, total %ADI was 1.262%, but the value has not effected on human health.

Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

Analysis of Methamphetamine and Amphetamine in Oral Fluid of Eleven Drug Abusers (마약남용자 11명의 타액 중 메스암페타민의 분석)

  • Kim, Eun-Mi;Lee, Ju-Seon;Choi, Hye-Young;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.419-425
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    • 2008
  • A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1497-1504
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    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

Polycyclic Aromatic Hydrocarbons in Agricultural Waterways in Gyeonggi and Gangwon Provinces, Korea (경기 및 강원지역 농업용수 중 PAHs의 모니터링 연구)

  • Kim, Leesun;Park, Byung-Jun;Lee, Sung-Eun
    • Korean Journal of Environmental Biology
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    • v.34 no.3
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    • pp.216-221
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    • 2016
  • Level and distribution of fourteen polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples collected in the waterways located in Gyeonggi and Gangwon, Korea were determined for monitoring and risk assessment. A simplified, fast but effective extraction and clean-up methods combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was employed to measure the concentration of the target compounds. The extraction of the analytes of interest in water sample (10 mL) was performed with acetonitrile (10 mL) and the salt. To purify the target PAHs, the clean-up procedure was employed with 2 mL tubes of dispersive solid phase extraction. The optimized method was validated with recoveries, method detection limit (MDL), accuracy and precision. Good recoveries for each PAHs at 10 and $25{\mu}g\;L^{-1}$ were achieved (60 to 110%, with RSD <20%) with linearity (>0.99). MDL for all the analytes was achieved with $0.2{\mu}g\;L^{-1}$. GC-MS/MS results showed that concentration of phenanthrene in the water samples from Gyeonggi (20 sites) ranged from 0.82 to $2.56{\mu}g\;L^{-1}$ and from Gangwon (15 sites) ranged from 0.83 to $1.62{\mu}g\;L^{-1}$. Other PAHs were not found in the water samples but the continuous monitoring for these areas were required.