• 제목/요약/키워드: (GC-MS) gas chromatography-mass spectrometry analysis

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A Scientific Analysis of Decorative Metal Foil Used in Pouch for the Sutra Embroidered with a Sun and Moon Design Designated as National Folklore Cultural Heritage (국가민속문화재 일월수 다라니 주머니 금속 장식지의 과학적 분석)

  • Pak, Seonghee;Park, Serin;Seo, Jeong Hun;Park, Jongseo;Lee, Ryangmi
    • Journal of Conservation Science
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    • v.38 no.2
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    • pp.124-132
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    • 2022
  • Through scientific analysis, this study identified the material characteristics of metal foil decorating the border line and knotting of the National Folklore Cultural Heritage 'Pouch for the Sutra Embroidered with a Sun and Moon Design'. Through Scanning Electron Microscope-Energy Dispersive Spectroscopy results, it was estimated that silver (Ag) and sulfur (S) were present in the metal foil, and silver leaf was also attached to the medium. S may discolor Ag from yellow to black depending on its concsentration and contact time. Yellow color could not be identified in metal foil at present. But there existed an example of the preparation of a gold-colored flat silver thread; therefore, further research is needed to estimate the original color. The lamella was reddish brown on the back. Aluminum, silicon, and iron were also detected and were the main components found in red soil. This is believed to be the red adhesive in traditional flat gold thread and is considered to be an adhesive-related component of the metal foil. From the gas chromatography mass spectrometry results, the adhesive component was confirmed to be animal glue.

Monitoring of Residual Pesticides and Exposure Assessment of Olive Oil Products Sold on the Market (올리브유의 잔류농약 모니터링 및 노출량 조사)

  • Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.4
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    • pp.211-216
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    • 2023
  • A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

Validity Assessment of Self-reported Smoking Status: Results from the Korean National Environmental Health Survey (KoNEHS) 2009-2011 (흡연상태에 관한 자가보고 설문의 타당도 평가: 제1기(2009-2011) 국민환경보건기초조사 자료 분석)

  • Choi, Wookhee;Park, Kyung Hwa;Kim, Hyun Jeong;Ryu, Jungmin;Yu, Seung Do;Choi, Kyunghee;Kim, Suejin
    • Journal of Environmental Health Sciences
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    • v.40 no.6
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    • pp.492-501
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    • 2014
  • Objectives: The purpose of this study was to assess the validity of self-reported cigarette smoking status and investigate factors associated with the accuracy self-reported and measured urinary cotinine in Korean adults. Methods: We used data from the $1^{st}$ Korean National Environmental Health Survey (2009-2011) among adults aged ${\geq}19$ years (N=6,246). The survey examined self-reported smoking status, and urinary cotinine was regarded as the biomarker of exposure to tobacco smoke. Urinary cotinine was analyzed using a gas chromatography-mass spectrometry (GC/MS) and data analysis was conducted using IBM SPSS version 20.0, which uses the sample weight and calculates variance estimates to adjust for the unequal probability of selection into the survey. Results: We calculated a cut-off point (53.3 ug/L) by using a ROC (Receiver Operating Characteristic) curve. The smoking prevalence was 24.6% based on self-reported data and 28.2% based on urinary cotinine concentrations. When we assessed the agreement between self-reported and urinary cotinine, we found an average agreement of 97.7% among self-reported smokers and 94.5% among self-reported non-smokers. Among self-reported smokers, factors affected the discrepancy were age, household economic status and average number of cigarettes smoked per day. On the other hand, gender, former smoking experience, and exposure to SHS (second hand smoke) were associated with discrepancies among self-reported non-smokers. Conclusion: These results suggest that self-reported data on smoking status provide a valid estimate of actual smoking status. In future research, we will conduct a continuous monitoring study for reliability verification of the data to reduce potential interpretation errors.

Comparison of isoButoxycarbonyl derivatives, tert.-butyldimethylsilyl derivatives, with US EPA Method in the sensitivity of Alkylphenols, Chlorophenols, and Bisphenol A Potential field-screening applications of GC/MS-SIM (기체 크로마토그래피/질량분석기를 이용한 field-screening 적용을 위한 알킬페놀류, 클로로페놀류 및 비스페놀 A의 isoBOC 유도체, TBDMS 유도체와 US EPA 방법의 비교)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.196-213
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    • 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.

Volatile Flavor Properties of Hallabong Grown in Open Field and Green House by GC/GC-MS and Sensory Evaluation (노지 및 시설에서 재배된 한라봉의 기기분석 및 관능평가에 의한 향기특성)

  • Song, Hee-Sun;Park, Yeon-Hee;Moon, Doo-Gyung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.8
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    • pp.1239-1245
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    • 2005
  • Hallabong peel oils grown in open field and green house were extracted by hand-pressing flavedo and collected on ice. Volatile flavor components of Hallabong peel oils were identified and compared by using gas chromatography and mass- spectrometry. Forty-four flavor components were identified in open field oil and 45 flavor components in green house oil. (E) -Limonene-1,2-epoxide and neral were identified only in Hallabong oil grown in open field, on the other hand, $\beta$-cubebene, $\beta$-elemene and decyl acetate were detected only in green house oil. Limonene was the most abundant component in both oils as more than 86$\%$ of peak weight, followed by sabinene (1.8$\~$ 3.6$\%$) and myrcene (2.4$\~ $2.6$\%$). The difference of the volatile profile between open field and green house oils were significantly characterized by identification and quantity of alcohol group. The total alcohols in open field and green house oils accounted for 1.8$\%$ and 0.8$\%$, respectively. Among alcohols, the level of linalool was relatively high in open field oil (1.2$\%$), however, it accounted for 0.5$\%$ in green house oil. Flavor properties of fresh Hallabong peel and flesh were also examined by sensory evaluation. Flavor properties of fresh Hallabong grown in open field were relatively stronger on both peel and flesh by sensory analysis. Sweetness was strong in Hallabong flesh from open field, and sourness in that from green house. The sensory evaluation of the preference in consideration of taste and aroma was significantly high in Hallabong grown in open field (p<0.01). From the present study, the stronger flayer properties and the preference of Hallabong from open field by sensory evaluation seem to be associated with the high level of linalool in its peel oil, and the composition of monoterpene hydrocarbons such as sabinene and (E) -$\beta$ -ocimene.

The analysis of ethylene glycol and metabolites in biological specimens (생체시료에서 에틸렌 글리콜과 그 대사체 분석에 관한 연구)

  • Park, Seh-Youn;Kim, Yu-Na;Kim, Nam-Yee
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.69-77
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    • 2011
  • Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

Fatty acid analysis and regulatory effects of citron (Citrus junos Sieb. ex TANAKA) seed oil on nitric oxide production, lipid accumulation, and leptin secretion (유자씨유의 지방산분석 및 Nitric Oxide 생성, 지방축적능, 렙틴분비 조절효과)

  • Kim, Tae Woo;Kim, Kyoung Kon;Kang, Yun Hwan;Kim, Dae Jung;Choe, Myeon
    • Journal of Nutrition and Health
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    • v.47 no.4
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    • pp.221-228
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    • 2014
  • Purpose: Citron seed oil (CSO) has been reported to have high antioxidant activity. However, the composition and other biologically activities of CSO have not been reported. In this study, we confirmed the fatty acid composition of CSO, which may be beneficial to vascular disease and obesity. Methods: We investigated the oil composition of CSO using gas chromatography coupled with mass spectrometry (GC-MS) analysis, and cytotoxicity was confirmed by Cell Counting Kit-8 (CCK-8) assay. Nitric oxide (NO) production in human umbilical vein endothelial cells (HUVECs) was measured using Griess reagent, and lipid accumulation and leptin secretion in 3T3-L1 cells were measured by Oil-Red O staining and commercial ELISA kit, respectively. Results: GC-MS analysis indicated that CSO contains several components, including linoleic acid, oleic acid, palmitic acid, stearic acid, linolenic acid, palmitoleic acid, and arachidic acid. In physiological activity analysis, CSO did not induce cytotoxic effects in HUVECs and 3T3-L1 cells. Further, CSO significantly induced nitric oxide and leptin secretion as well as inhibited lipid accumulation. Conclusion: CSO increased NO release, inhibited lipid accumulation, and induced leptin secretion, suggesting it may be useful for the management of vessels and weight gain. Although further studies are required to investigate the safety and mechanism of action of CSO, our results show that the composition and physiological activity of CSO are sufficient for its use as functional edible oil.

Translocation of Tolclofos-methyl from Ginseng Cultivated Soil to Ginseng (Panax ginseng C. A. Meyer) and Residue Analysis of Various Pesticides in Ginseng and Soil (토양 중 잔류된 Tolclofos-methyl의 인삼(Panax ginseng C. A. Meyer)에 대한 이행 및 잔류 특성)

  • Kim, Ji Yoon;Kim, Hea Na;Saravanan, Manoharan;Heo, Seong Jin;Jeong, Haet Nim;Kim, Jang Eok;Kim, Kwan Rae;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.130-140
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    • 2014
  • Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

Analysis of the Component and Immunological Efficacy of Chamaecyparis obtusa Leaf Extract (편백나무 잎 추출물의 성분분석과 면역효능에 관한 연구)

  • Kim, Joung Hee;Lee, Syng-Ook;Do, Kook Bae;Ji, Won Dae;Kim, Sun Gun;Back, Young Doo;Kim, Keuk-Jun
    • Korean Journal of Clinical Laboratory Science
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    • v.50 no.1
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    • pp.37-43
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    • 2018
  • Chamaecyparis obtusa (CO) has recently been attracting attention because of its beneficial effects on skin allergies, atopic dermatitis, and skin diseases, such as acne and eczema. In the present study, the extract from CO leaf grown in Jangseong gun, Jeollanam-do, Korea was evaluated for its anti-oxidant, anti-inflammatory, and anti-allergic effects in vitro. The total polyphenol content of the CO leaf extract was $25.89{\pm}0.31mg$ gallic acid equivalents (GAE)/g. Gas-chromatography mass-spectrometry (GC-MS) analysis revealed the presence of six compounds in the CO leaf extract: ${\alpha}-terpinene$ (3.03 mg/g), ${\alpha}-terpineol$ (9.48 mg/g), limonene (5.96 mg/g), borneol (59.78 mg/g), myrcene (4.85 mg/g), and sabinene (11.31 mg/g). The $RC_{50}$ values of the CO leaf extract for $H_2O_2$ and ABTS radical were $5.47{\pm}0.13mg/mL$ and $4.00{\pm}0.01mg/mL$, respectively. In addition, the CO leaf extract showed significant inhibitory effects on lipopolysaccharide-induced nitric oxide production in RAW 264.7 cells and IgE-induced release of ${\beta}-hexosaminidase$ (degranulation) in mast-cell like RBL-2H3 cells. The cell viability assay showed that the CO leaf extract ($100{\sim}800{\mu}g/mL$) did not affect the viability of human normal skin fibroblast CCD-986sk cells significantly. Overall, these results suggest that the CO leaf extract is a potential functional cosmetic ingredient that can exert anti-oxidant, anti-inflammatory, and anti-allergic effects.