• Title/Summary/Keyword: GC and GC-MS method

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Study on analysis of PAHs in consumer products (공산품 함유 PAHs 분석법에 관한 연구)

  • Song, Moon Hwan;Cho, Young Dal;Choe, Eun Kyung
    • Analytical Science and Technology
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    • v.27 no.4
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    • pp.201-212
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

Separation of Chromophoric Substance from Sappanwood under Different Extraction Conditions (염료 추출조건에 따른 소목의 색소성분 분리 거동)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.31 no.12
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    • pp.1653-1661
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    • 2007
  • The research aimed to establish the standard extraction procedure for examining brazilin, the major chromophoric substance of Sappanwood, using GC-MS with the ultimate goal of identifying the sappanwood dye in severely faded archaeological textiles. The amount of brazilin represented by the GC abundance was the largest when acetone was used as the extraction medium, followed by methanol. Shaking plate operated at room temperature was more effective than the waterbath shaker which was operated at $30^{\circ}C$. In both cases, the extraction method which incorporated one hour pre-soaking before the 12 hours of actual extraction resulted in a larger amount of brazilin detection than the extraction procedure without the one hour pre-soaking. In case of water extraction, pH 5 resulted in the most effective pH level for the extraction of brazilin, The best GC-MS parameter for detecting brazilin was to set the column temperature initially at $50^{\circ}C$. gradually increase to $210^{\circ}C$ at a $23^{\circ}C/min$ rate, finally increase to $305^{\circ}C$ at $30^{\circ}C/min$ rate, and hold for 14 minutes, and the MSD scan range at $75{\sim}400m/z$.

Analysis of toluene diisocyanate of adhesives in food contact materials by GC/MS (GC/MS에 의한 식품 포장재에 사용되는 접착제의 Toluene diisocyanate 분석)

  • Oh, Chang-Hwan;Kim, Ji-Young;Jo, Cheon-Ho;Park, Heera;Kwun, Ki-Sung;Kim, Meehye;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.18 no.6
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    • pp.511-519
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    • 2005
  • A method for determination of toluene diisocyanates (TDI) in toluene diisocynate (TDI)-based polyurethane (PUR) packing material was investigated, and also the migration of TDI to food was studied. TDI was extracted using food simulants such as n-haptane and 4% aqueous acetic acid. The determinations were performed using gas chromatography/mass spectrometry (GC/MS). One of major components for polyurethane, toluene diisocyanates, were detected in ten samples among twenty six food contact materials with the concentration range of $0.51{\sim}60.88{\mu}g/ml$. However the highest extracted amount was just 0.7% of $60.88{\mu}g/ml$ if the contact surface of food packing for extracting liquid was limited to the outer layer without exposure of the cutting edge of food packing multi-layers. The result of this study and the analysis method for TDI diisocyanate will be very useful for further study about food contact material, and the monitoring result could be used for evaluating the safety of food contact material before it is to be used for food, preservation.

Development of a GC-MS Diagnostic Method with Computer-aided Automatic Interpretation for Metabolic Disorders (GC-MS 크로마토그램의 컴퓨터 자동해석을 이용한 유전성 대사질환의 진단법 개발)

  • Yoon, Hye-Ran
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.6 no.1
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    • pp.40-51
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    • 2006
  • Purpose: A personal computer-based system was developed for automated metabolic profiling of organic aciduria and aminoacidopathy by gas chromatography-mass spectrometry and data interpretation for the diagnosis of metabolic disorders Methods: For automatic data profiling and interpretation, we compiled retention time, two target ions and their intensity ratio for 77 organic acids and 13 amino acids metabolites. Metabolites above the cut-off values were flagged as abnormal compounds. The data interpretation was a based on combination of flagged metabolites. Diagnostic or index metabolites were categorized into three groups, "and", "or" and "NO" compiled for each disorder to improve the specificity of the diagnosis. Groups "and" and "or" comprised essential and optional compounds, respectively, to reach a specific diagnosis. Group "NO" comprised metabolites that must be absent to make a definite diagnosis. We tested this system by analyzing patients with confirmed Propionic aciduria and others. Results: In all cases, the diagnostic metabolites were identified and correct diagnosis was founded to be made among the possible disease suggested by the system. Conclusion: The study showed that the developed method could be the method of choices in rapid, sensitive and simultaneous screening for organic aciduria and amino acidopathy with this simplified automated system.

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Comparison of GC-Profile on Tobacco Smoke Components (담배 연기성분의 GC-Profile 특성비교)

  • 나효환;한상빈;복진영;이운철;백순옥;장기철;양광규
    • Journal of the Korean Society of Tobacco Science
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    • v.16 no.2
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    • pp.152-162
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    • 1994
  • This study was designed to establish an analytical method for the properties of leaf tobacco smoke. Lyophilized TPM from leaf tobacco smoke was extracted with MeOH, dried under reduced pressure, and trimethyl-silylated(TMS). Gas chromatography of the material using SPB-5 column showed 120 quantifiable peaks. Among those, 26 compounds including a hydrocarbons, Neophytadiene. and Levulinic acid could be identified through GC-MS. Smoke properties of 5 manufacturing grades and 2 oriental cultivars of domestic and imported leaf tobacco including AB3O-1 were analyzed. For flue-cured tobacco, content of the compounds in the smoke was generally higher in American leaf tobacco except for glycerol compounds. For burley tobacco, domestic leaves were found to have much higher amount of smoke compound than imported leaves. Among oriental tobacco, Izmir contained slightly higher amount of smoke compounds than Basma. Key words : GC - profile. TPM. TMS. Leaf tobacco.

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Comparative Sampling Procedures for the Volatile Flavor Components of Codonopsis lanceolata (전처리 방법에 따른 더덕(Codonopsis lanceolata)의 휘발성 향기성분 비교 분석)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Kim, Jae-Jung;Oh, Chang-Hwan
    • Korean Journal of Food Science and Technology
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    • v.24 no.2
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    • pp.171-176
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    • 1992
  • Volatile flavor components of Codonopsis lanceolata were extracted by gas co-distillation (GCD), solvent extraction/fractionation (SEF), and headspace sampling (HSS) methods. The extracts were analyzed by dual-capillary gas chromatography-retention index (GC-RI) and gas chromatography-mass spectrometry(GC-MS). The two extracts prepared by SEF and HSS gave more similar fragrance to the Codonopsis lanceolata than the GCD extract. The GC profiles of the SEF and HSS extracts were similar to each other except for differences in peak areas. The extract prepared by SEF gave a sweet note while the extract prepared by HSS gave a green note. The GCD extract began to give a burnt note of herb medicine with prolonged distillation. Rapid extraction of flavor components from Codonopsis lanceolata was possible in several short steps by SEF and HSS methods compared to GCD. GC-MS and GC-RI were used for peak identification. GC-RI was more effective for identification of isomers, and polar FFAP column was more suitable for identification of polar compounds. From Codonopsis lanceolata we identified 35 volatile flavor constituents, 24 of which have not been previously reported by simultaneous distillation extraction method $^{(5)}$. trans-2-Hexanal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, and hexanol were considered key components of the green note and 1-octen-3-ol, the component of the fresh note. Esters, including amyl propionate, seem to be responsible for the sweet note particular to Codonopsis lanceolata.

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Examination about evaluation method of odor active compounds in evaporator by using condensed water (응축수를 이용한 냉각기의 냄새원인물질 평가방법 검토)

  • Kim, Sun-Hwa;Kim, Kyung-Hwan;Jung, Young-Rim;Kim, Man-Goo;Kim, Jae-Ho;Park, Ha-Young;Ji, Yong-Jun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.361-369
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    • 2007
  • Uncomfortable odor emitted from air conditioning system is the main cause of indoor air quality deterioration. To solve evaporator odor problems, odor active compounds, have to be identified then the quality of the product can be improved its quality. Because evaporator odor in exhaust gas has low odor intensity and discontinuity, it is very difficult to collect and analyze sample. In this study through the identification of odor compounds in condensed water, the evaluation of the eraporator was tested. Odor compounds were extracted from water by headspace-solid-phase microextraction (HS-SPME) method. The single odor was separated by GC/FID/Olfactometry (GC/FID/O) and odor active compounds were identified by GC/AED and GC/MS. Compared to air sample, result of sensory evaluation and the single odor compound appeared similarly. It was identified that odor active compounds have functional group containing oxygen such as alcohols and acids. Evaluation method of odor active compounds using condensed water in evaporator appeared effective on the side of simplicity of collection, low expanse and rapid analysis.

Development and Validation of an Analytical Method for Flutianil Residue Identification Using Gas Chromatography-Electron Capture Detection (GC-ECD를 이용한 flutianil 잔류량 분석법 개발 및 확인)

  • Kwon, Ji-Eun;Do, Jung-Ah;Park, Hyejin;Lee, Ji-Young;Cho, Yoon-Jae;Oh, Jae-Ho;Rhee, Gyu-Seek;Lee, Sang-Jae;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.46 no.1
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    • pp.7-12
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    • 2014
  • A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

Detection Characteristics of Gamma-Irradiated Seeds by using PSL, TL, ESR and GC/MS (PSL, TL, ESR 및 GC/MS 분석을 통한 감마선 조사된 유지종실류의 검지 특성 연구)

  • Kim, Kyu-Heon;Son, Jin-Hyok;Kang, Yoon-Jung;Park, Hye-Young;Kwak, Ji-Young;Lee, Jae-Hwang;Park, Yong-Chjun;Jo, Tae-Yong;Kim, Jae-I;Lee, Hwa-Jung;Lee, Sang-Jae;Han, Sang-Bae
    • Journal of Food Hygiene and Safety
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    • v.28 no.2
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    • pp.130-137
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    • 2013
  • In this study, we investigated the applicability of the photostimulated luminescence (PSL), thermoluminescence (TL), electron spin resonance (ESR) and gas chromatography/mass spectrometry (GC/MS) methods for 5 seeds which are not allowed to be irradiated in Korea. All 5 seeds including evening primrose seed, safflower seed, rape seed, sunflower seed and flax seed were analyzed. Samples were irradiated at 1~10 kGy using a $^{60}Co$ gamma-ray irradiator. In PSL study, the photon counts of all the unirradiated samples showed negative (lower than 700). The photon counts of irradiated (1, 5, 10 kGy) samples showed positive (higher than 5,000). In TL analysis, results showed that it is possible to apply TL method to all foods containing minerals. In ESR measurements, the ESR signal (single-line) intensity of irradiated foods was higher than non-irradiated foods. The hydrocarbons 1,7-hexadecadiene ($C_{16:2}$) and 8-heptadecene ($C_{17:1}$) from oleic acid were detected only in the irradiated samples before and after the treatment at doses ${\geq}$ 1 kGy, but they were not detected in non-irradiated samples before and after treatment. These two hydrocarbons could be used as markers to identify irradiated safflower seed, rape seed, Sunflower seed and flax seed. And then, the hydrocarbons 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$) from linoleic acid were detected in the evening primrose seed, safflower seed and sunflower seed. According to the results, PSL, TL and GC/MS methods were successfully applied to detect the irradiated foods. It is concluded that PSL, TL and GC/MS methods are suitable for detection of irradiated samples and a combined method is recommendable for enhancing the reliability of detection results.

디클로벤지딘에 폭로된 흰쥐의 간장세포와 방광 상피세포에 형성된 DNA adducts의 $^{32}P-postlabeling$과 GC/MS-SIM에 의한 분석

  • 이진헌;신호상;장미선
    • Proceedings of the Korean Environmental Health Society Conference
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    • 2002.04a
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    • pp.49-51
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    • 2002
  • To identify and evaluate the dichlorobenzidine(DCB)-DNA adducts in liver cell and bladder epithelial cells by $^{32}$ P-postlabeling and GC/MS-SIM, we orally exposed the dichlorobenzidine (20mg/kh body wt.,/day)to male sprague-dawley rats for 14 days. Two kinds of DCB-DNA adduct were found at the same site of thin layer chromatogram of $^{32}$ P-postlabeling method in liver cells and bladder epithelial cells. In liver cells, relative adduct labeling(RAL) $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 34.1$\pm$3.71 and 69.9$\pm$5.02, that of adduct A2 were 74.1$\pm$10.1 and 105.1$\pm$10.1 on 10 and 14 days after treatment, respectively. And in bladder epithelia cells, RAL $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 5.92$\pm$1.60 and 15.9$\pm$1.31, that of adduct A2 were 9,81$\pm$2.81 and 22.8$\pm$1.79 on 10 and 14 days after treatment, respectively. DCB metabolites formed DNA adducts were monoacetyl-dichlorobenzidine(acDCB) and diacety1-dichlorobenzidine(di-acDCB), which was identify by gas chromatography/mass spectrometry-scan ionization mode(GC/MS-SIM), along with hydrolysis, extraction and TFA(trifluoroacetyl anhyride) derivatization with DCB-DNA adducts isolated from live cells and bladder epithelial cells. The base peak of acDCB were 252 and 294 m/z, and that of di-acDCB were 252, 294 and 336 m/z. In conclusion, the exposed DCB formed two kinds of DCB-DNA adduct, the proximate materials of that were acDCB and di-acDCB in liver and bladder epithlial cells. And the above GC/MS-SIM method was found the DCB-DNA adducts could be monitoring by gas chromatography.

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