• Title/Summary/Keyword: gas chromatography-mass spectrometry

Search Result 989, Processing Time 0.031 seconds

Case Study on Determination of the Level of New RoHS II Substances in Domestic Electronic and Electrical Equipments (국내 전기전자 제품에 함유된 신규 RoHS II 물질 검출 사례 연구)

  • Song, Moon-Hwan;Son, Seung-Hwan;Cho, Young-Dal;Choe, Eun-Kyung
    • Clean Technology
    • /
    • v.17 no.2
    • /
    • pp.124-133
    • /
    • 2011
  • In addition to six substances regulated in EU RoHS including lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE), priority substances are identified in new RoHS II as hexabromocyclododecane (HBCDD), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP) and diethylhexyl phthalate (DEHP). In this study, 20 plastic samples were collected from 12 domestic electrotechnical companies and levels of four restricted substances were determined by gas chromatography-mass spectrometry, Among 20 parts that compose washer, refrigerator or microwave oven, HBCDD was detected in three samples of NBR material with the amount of 42~381 mg/kg while DBP and BBP was not detected in any samples collected respectively, implying that these substance may not be used widely in plastic materials for EEE. However, DEHP was detected in all samples of NBR, PP, PBT, EPDM and PVC materials with the amount of 42 up to 59,400 mg/kg that exceeds the limit value of 0.1 wt% (1,000 mg/kg). Presence of a restricted substance in polymer material makes a great negative influence on a number of final product. To cope with coming RoHS II as well as REACH, action not to use DEHP in plastic material or the relevant notification in case of REACH seems to be needed. Screening test of Arsenic compounds such as diarsenic pentaoxide, diarsenic trioxide, lead hydrogen arsenate, triethyl arsenate that are included in REACH SVHC was done by ICP measurement Arsenium was detected in four samples made of NBR and PBT materials in the level of 15~700 mg/kg. By considering the screening method used in this study, the amount of arsenium compounds in the thermistor made of PBT material has a high chance of exceeding the regulated limit value.

A Survey on Endocrine Disrupting Chemicals in Animal Wastes Treated with Methane Fermentation (메탄발효 처리된 가축분뇨내의 내분비계 장애물질에 대한 조사 연구)

  • Ko, H.J.;Kim, K.Y.;Kim, H.T.;Umeda, M.
    • Korean Journal of Environmental Agriculture
    • /
    • v.26 no.1
    • /
    • pp.62-68
    • /
    • 2007
  • Concerns about endocrine disrupting chemicals emitted from humans and animals have been increased because these compounds are detected at very low levels in environment and adversely affect on indigenous fauna. To date, there is little information regarding the concentration of these compounds in animal wastes. In this study, the female hormones, $17\beta-estradiol$ (E2), estrone (E1) and estriol, were measured to provide baseline data in animal wastes. Samples were collected from animal waste storage, methane digester and sludge separated wastewater and analyzed by gas chromatography-mass spectrometry. To measure the mass ratios of estrogen to macronutrients, nitrogen and phosphorous were also determined. Sample collected from animal waste storage had the highest estrogen concentration (98.7 ${\mu}g/L$), while sludge separated wastewater had the lowest concentration (3.4 ${\mu}g/L$). The mean concentrations of E2 and E1 in waste storage sample were (6.8 ${\mu}g/L$) and (68.7 ${\mu}g/L$), respectively. In sludge separated wastewater, the mean concentration of both E2 and E1 were reduced to (2.6 ${\mu}g/L$) and (1.9 ${\mu}g/L$), respectively. However, estriol was not detected in any of the samples collected. Mean ratios of E2 and E1 to macronutrients were significantly different between the methane wastewater and sludge separated wastewater owing to elimination of solid particles.

The Monitoring on Plasticizers and Heavy Metals in Teabags (침출용 티백 포장재의 안전성에 관한 연구)

  • Eom, Mi-Ok;Kwak, In-Shin;Kang, Kil-Jin;Jeon, Dae-Hoon;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Hee-Jung;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
    • /
    • v.21 no.4
    • /
    • pp.231-237
    • /
    • 2006
  • Nowadays the teabag is worldwide used for various products including green tea, tea, coffee, etc. since it is convenient for use. In case of outer packaging printed, however, there is a possibility that the plasticizers which is used for improvement in adhesiveness of printing ink may shift to inner tea bag. In this study, in order to monitor residual levels of plasticizers in teabags, we have established the simultaneous analysis method of 9 phthalates and 7 adipates plasticizers using gas chromatography (GC). These compounds were also confirmed using gas chromatography-mass spectrometry (GC-MSD). The recoveries of plasticizers analyzed by GC ranged from 82.7% to 104.6% with coefficient of variation of $0.6\sim2.7%$ and the correlation coefficients of each plasticizer was $0.9991\sim0.9999$. Therefore this simultaneous analysis method was showed excellent reproducibility and linearity. And limit of detection (LOD) and limit of quantitation (LOQ) on individual plasticizer were $0.1\sim3.5\;ppm\;and\;0.3\sim11.5\;ppm$ respectively. When 143 commercial products of teabag were monitored, no plasticizers analysed were detected in filter of teabag products. The migration into $95^{\circ}C$ water as food was also examined and the 16 plasticizers are not detected. In addition we carried out analysis of heavy metals, lead (Pb), cadmium (Cd), arsenic (As) and aluminum (Al) in teabag filters using ICP/AES. $Trace\sim23{\mu}g$ Pb per teabag and $0.6\sim1718{\mu}g$ Al per teabag were detected in materials of samples and Cd and As are detected less than LOQ (0.05 ppm). The migration levels of Pb and Al from teabag filter to $95^{\circ}C$ water were upto $11.5{\mu}g\;and\;20.8{\mu}g$ per teabag, respectively and Cd and As were not detected in exudate water of all samples. Collectively, these results suggest that there is no safety concern from using teabag filter.

An Improved Analytical Method for the Determination of Qualitative and Quantitative Characteristics of Di- and Trisaccharides in Honey using GC and GC/MS (GC 및 GC/MS에 의한 벌꿀 중의 이·삼당류 정성 및 정량 특성과 개선된 동시분석방법의 확립)

  • Kim, Jong-Bae;Jang, Eun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Seo, Hyun-Sun;Park, Nam-Pyo
    • Korean Journal of Food Science and Technology
    • /
    • v.47 no.1
    • /
    • pp.27-36
    • /
    • 2015
  • The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.

Chemical Composition and Antiproliferative Activity of Supercritical Extract of Immature Citrus Peel in human cervical carcinoma HeLa cells (미성숙 감귤 과피 초임계 추출물의 성분 분석과 자궁암세포 성장억제효능)

  • Moon, Jeong Yong;Song, YeonWoo;Hyun, Ho Bong;KimCho, Somi
    • Journal of the Korea Academia-Industrial cooperation Society
    • /
    • v.16 no.12
    • /
    • pp.8836-8843
    • /
    • 2015
  • This study was performed to investigate the antiproliferative activities of supercritical extracts from phalsak(Citrus hassaku Hort ex Tanaka) and yeagam(Citrus iyo Hort. ex Tanaka) against human cervical carcinoma HeLa cells and the chemical compositions of the extracts. The anticancer properties of supercritical extracts were demonstrated using the MTT assay and Hoechst 33342 staining and the compositional analyses were conducted by using gas chromatography-mass spectrometry(GC-MS). The peel extracts of both species exhibited similar antiproliferative effect. The antiproliferative activity of the flesh extracts was not detected up to $400{\mu}g/mL$, whereas peel extracts of phalsak and yeagam reduced cell viability with 87.16% and 92.95% at $400{\mu}g/mL$, respectively. There was a dramatic increase of the apoptotic body formation in the cell treated with peel extracts while no apoptotic body formation detected in the cell treated with flesh extracts at 100, $200{\mu}g/mL$. By GC-MS analysis, 27 and 31 kinds of compounds identified in flesh and peel of phalsak, while 27 and 29 kinds of compounds were identified in flesh and peel of yeagam, respectively. 1,1,4,4-Tetramethyl-2-tetralone(20.86%), alloimperatorin(8.15%), limonene(11.23%), and auraptene(7.29%) were major in peel of phalsak, whereas limonene(22.19%), linalool(11.23%), and ${\gamma}$-sitosterol(9.12%) were major in peel of yeagam.

Composition and Cell Cytotoxicity of Essential Oil from Caryopteris incana Miq. in Korea (층꽃나무(Caryopteris incana Miq) 정유의 성분 분석과 세포 독성 평가)

  • Kim, Song-Mun
    • Applied Biological Chemistry
    • /
    • v.51 no.3
    • /
    • pp.238-244
    • /
    • 2008
  • The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

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
    • /
    • v.50 no.1
    • /
    • pp.37-43
    • /
    • 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.

Determination of homogentisic acid in human plasma by GC-MS for diagnosis of alkaptonuria (GC-MS를 이용한 혈장 중 호모겐티식산의 분석;알캅톤뇨증의 진단)

  • Thapa, Maheshwor;Yu, Jundong;Lee, Wonjae;Islam, Fokhrul;Yoon, Hye-Ran
    • Analytical Science and Technology
    • /
    • v.28 no.5
    • /
    • pp.323-330
    • /
    • 2015
  • Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

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
    • /
    • v.24 no.2
    • /
    • pp.69-77
    • /
    • 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.

Emission characteristics of volatile organic compounds released from spray products (생활 스프레이 제품의 안전성 조사: 벤젠과 톨루엔 함량을 중심으로)

  • Jo, Hyo-Jae;Kim, Bo-Won;Kim, Yong-Hyun;Lee, Min-Hee;Jo, Sang-Hee;Kim, Ki-Hyun;Kim, Joon-Young;Park, Jun-Ho;Oh, Soo-Min;Lee, Seung-Hwan;Kim, Dong-Yeon
    • Analytical Science and Technology
    • /
    • v.26 no.4
    • /
    • pp.268-275
    • /
    • 2013
  • Many kinds of liquid spray products are used in livelihood activities these days. Spray products can be distinguished by the target to be sprayed (like into the air or on human skin (body)). Because human can be exposed to volatile organic compounds (VOC) emitted from spray products, some considerations on safety or hazard of spray products should be needed. In this study, emission characteristics of VOCs were investigated against 10 types of liquid spray products (6 skin spray and 4 air spray products). The concentrations of benzene and toluene were determined by gas chromatography/mass spectrometry (GC/MS) equipped with a thermal desorber (TD). Their average concentrations from 6 skin spray products exhibited$ 5.64{\pm}1.95$ ($mean{\pm}S.D$) and $8.52{\pm}2.89$ ppb(w), respectively. In contrast, those of 4 air spray samples had $7.30{\pm}1.31$ and $7.19{\pm}1.78$ ppb(w), respectively. If liquid contents in spray samples are completely vaporized in one cubic meter (1 m3) after spraying for 10 seconds, their mean concentrations of skin spray products are $31.7{\pm}8.80$ (benzene) and $50.5{\pm}17.1{\mu}g/Sm^3$ (toluene). In contrast, those of air spray products are $24.0{\pm}4.30$ (benzene) and $23.6{\pm}5.83{\mu}g/Sm^3$ (toluene). The estimated concentration levels of benzene from two types of products (31.7 and $24.0{\mu}/Sm^3$) exceeded the Korean atmospheric environmental guideline ($5{\mu}g/Sm^3$). The results of this study thus suggest that some measures should be made to reduce or suppress the contents of VOC in spray products.