• Title/Summary/Keyword: headspace GC method

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Analysis of Flavor-related Compounds from Tobacco using SPME-GC-MS (SPME-GC-MS를 이용한 담배와 관련된 향료의 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.109-114
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    • 2001
  • The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry(GC-MS). Flavor-related compounds were estragole pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin. More than on of the flavor-related compounds were detected in the range $0.001-1.3{\mu}g/g$ from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%.

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Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.139-142
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    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

Establishment for analytical method of methanol in wet wipes by headspace gas chromatography (가스크로마토그래프-헤드스페이스를 이용한 물휴지 중 메탄올 정량법 확립 연구)

  • Choi, Yongkyu;Baek, Eunji;Min, Chungsik;Lee, Rheeda;Park, Soonyoung;Ahn, Jaehyung;Kim, Sangseop;Hong, Seonghwa;Kim, Younglim
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.242-247
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    • 2016
  • This research aims to set up and validate methods of analyzing the methanol in wet wipes and verifies the analysis methods that applied to the wet wipes. We used Headspace (HS) Gas Chromatography (GC) - Flame Ionization Detector (FID) to the establish analysis method of methanol in wet wipes and optimized heating temperature, heating time, GC conditions with column. The result indicated that 3 mL of sample in 20 mL headspace vial can be equilibrated efficiently in headspace sampler at 70 ℃ for 10 min and sample was measured by GC with spli injection mode(10:1). The results show that linearity from 1 to 100 ppm was over R2 0.9995, precision was RSD 1.83 % and accuracy(recovery rate) was 105.44 (±1.05 %) on water matrix and wet wipes matrix removed non-woven fabric. Also, monitoring results of total 20 cosmetics on the market, from 0.00017 to 0.00156 % of methanol was detected from wet wipes.

Volatile Components of Green Tea(Camellia sinensis L. var. Yabukita) by Purge and Trap Headspace Sampler (Purge와 Trap Headspace Sampler를 이용한 녹차의 휘발성 성분)

  • 이재곤;권영주;장희진;곽재진;김옥찬;최영현
    • The Korean Journal of Food And Nutrition
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    • v.10 no.1
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    • pp.25-30
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    • 1997
  • Volatile components of green tea were isolated by purge and trap headspace method and were analyzed by GC and GC/MSD. And ten headspace volatiles were compared with volatiles isolated by simultaneous distillation-extraction(SDE) method. A total of 99 components were identified in the green tea volatile components, from which 88 components were identified in the headspace volatiles, contained 20 alcohols, 30 hydrocarbons, 21 aldehydes, 10 ketones, 2 acids and 5 miscellaneous components. The major components were low boiling components, such as methyl butanal(3.1%), 1-penten-3-ol(5.48%), 2-penten-1-ol(2.89%), hexanal(5.77%), heptanal(1.90%), and ere 2,4-eptadienal(4.28%), linalool(2.27%), 2,6-dimethyl cyclohexanol(2.57%), $\alpha$-pinene(1.52%), caryophyllene(1.70%), and carbonyl compounds, such as $\alpha$-ionone(2.62%), $\beta$-ionone(2.98%), $\beta$-cyclocitral(2.0%). On the other hand SDE volatiles, from which 64 components were identified, contained 16 alcohols, 16 ydrocarbons, 15 aldehydes, 10 ketones, 3 acids and 4 miscellaneous components. The major components were alcohols, such as, benzyl alcohol(3.79%), linalool(9.52%), terpineol(2.16%), geraniol(2.75%), nerolidol(6.50%), ketones, such as $\alpha$-ionone(1.77%), $\beta$-ionone(4.80%), geranyl acetone(1.82%) and acids, such as hexanoic acid(1.45%), nonanoic acid(1.11%).

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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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Analysis of Benzene in Beverages by Headspace-GC/MS (Headspace-GC/MS를 이용한 음료 중 벤젠 분석)

  • Kim, Eun-Ju;Park, Sang-Aeh;Choi, Dong-Mi
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.243-247
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    • 2007
  • A selective analytical method of headspace-GC/MS has been applied to determine levels of benzene in beverages. Food samples were 85 including 2 fruit juices, 6 fruit beverages, 11 carbonated beverages, 55 mixed beverages, and 4 beverage concentrations, and 7 extracted beverages. For phase equilibration of headspace, sample was stirred at $40^{\circ}C$ for 30 min. The oven temperature was $60^{\circ}C$ and elevated to $180^{\circ}C$ at $15^{\circ}C/min$. The internal standard was benzene-d6. The identification was done by the selected target ions such as m/z 51, 77, and 78 and the confirmation was done by the response ratio of m/z 77 to m/z 78 between sample and standard. The overall recoveries were ranged from 91% to 101% and the limit of quantification was $1{\mu}g/kg$. The average level of benzene were $5{\mu}g/kg$ for fruit beverages, $2{\mu}g/kg$ for carbonated beverages, $7{\mu}g/kg$ for mixed beverages and $7{\mu}g/kg$ for extracted beverages.

The Analysis of Airborne Trimethylamine Using a Headspace (HS)-SPME Method (헤드스페이스-SPME 방법을 이용한 트리메틸아민의 분석방법 연구)

  • Ahn, Ji-Won;Kim, Ki-Hyun
    • Journal of Korean Society for Atmospheric Environment
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    • v.24 no.3
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    • pp.357-366
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    • 2008
  • In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

Determination of Volatile Organic Compounds in Waste using HS/GC/MS Analysis (Headspace/GC/MS를 이용한 폐기물중 휘발성 유기화합물의 분석)

  • Kim, Kyeo-Keun;Shin, Sun-Kyoung;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.72-80
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    • 2000
  • The HS/GC/MS method was performed to analyze the volatile organic compounds in waste sludge samples. This study was performed to establish the fundamental data by studying the effects of salt, equilibrium temperature and time in the volatile organic compounds analysis. The presence of salts have been found to increase the sensitivity. The peak area is increased from 1.07 to 2.61 times by adding the salts to the water sample, compared with a salt tree sample. The recoveries of target compounds have found between 90% and 127% at sample temperature of $85^{\circ}C$ for 30 min. This HS/GC/MS method can be applied to analyze the volatile organic compounds and organohalo compounds in the environmental matrix.

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Development of an Analytical Method for Chloropicrin Determination in Hulled Rice by GC-ECD and GC-MS (GC-ECD 및 GC-MS를 이용한 현미 중 chloropicrin의 잔류시험법 개발)

  • Do, Jung-Ah;Choi, Jeong-Heui;Park, Hyejin;Park, Yong-Chun;Yoon, Hae-Jung;Choi, Dongmi;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.28 no.3
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    • pp.222-226
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    • 2013
  • A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.