• Title/Summary/Keyword: headspace sample

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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 Compounds and Carotenes Analysis of Korean Beeswax (한국산 밀립의 휘발성 성분과 Carotene류의 분석)

  • Kwon, Hye-Soon
    • Journal of the Korean Applied Science and Technology
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    • v.15 no.4
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    • pp.63-69
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    • 1998
  • The beeswax sample was collected from the beehives, isolated and then refined. The first step of producing beeswax was to separate honey from beehives. The beehives which were cut put in hot water. The upper layer was crude beeswax, which was treated with phosphoric acid. The crude beeswax was purified through the bleaching. The objectives of this study are to identify headspace volatile compounds and to know the contents of ${\alpha}$-carotenes and ${\beta}$-carotenes of korean beeswax. Headspace volatile compounds of Korean beeswax were measured by using the combination of dynamic headspace sampler (DS 5000, Donam System Inc.), gas chromatography and mass selective detector (HP5890 & 5971, Hewlett Packard). Seventy five compounds identified from about 100 peaks by analyzing the purified beeswax were 60 hydrocarbons, 8 carbonyls, 4 essential oils, 3 esters. Carotenes of Korean beeswax were analyzed by using High Performance Liquid Chromatography (Waters Inc.). As A result, the content of ${\alpha}$-carotenes and ${\beta}$-carotenes were 0.07ppm, 0.011ppm individually.

Analysis of Flavor Composition of Coriander Seeds by Headspace Mulberry Paper Bag Micro-Solid Phase Extraction

  • Cha, Eun-Ju;Won, Mi-Mi;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2675-2679
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    • 2009
  • This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

Headspace GC-MS Analysis of Spring Blossom Fragrance at Chungnam National University Daedeok Campus

  • Choi, Yeonwoo;Lee, Sanghyun;Kim, Young-Mi;Nguyen, Huu-Quang;Kim, Jeongkwon;Lee, Jaebeom
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.125-132
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    • 2022
  • There are many types of spring blossoms on the Daedeok campus of Chungnam National University (CNU) at the area of 1,600,000 square meters. As an assignment for the class of Analytical Chemistry I for second-year undergraduate students, 2021, flower petals collected from various floral groups (Korean azalea, Korean forsythia, Dilatata lilac, Lilytree, Lily magnolia, and Prunus yedoensis) were analyzed using headspace extraction coupled to gas chromatography-mass spectrometry (HS-GC-MS) to study the aromatic profiles and fragrance compounds of each sample group. Various types of compounds associated with the aroma profiles were detected, including saturated alcohols and aldehydes (ethanol, 1-hexanol, and nonanal), terpenes (limonene, pinene, and ocimene), and aromatic compounds (benzyl alcohol, benzaldehyde). The different contribution of these compounds for each floral type was visualized using statistical tools and classification models based on principal component analysis with high reliability (R2 = 0.824, Q2 = 0.616). These results showed that HS-GC-MS with statistical analysis is a powerful method to characterize the volatile aromatic profile of biological specimens.

Volatile Component Analysis of Commercial Japanese Distilled Liquors (Shochu) by Headspace Solid-Phase Microextraction (헤드스페이스 고체상미량추출(Solid-Phase Microextraction)을 이용한 시판 일본소주의 휘발성 향기성분 분석)

  • Shin, Kwang-Jin;Lee, Seung-Joo
    • Korean Journal of Food Science and Technology
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    • v.47 no.5
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    • pp.567-573
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    • 2015
  • In this study, volatile compounds in nine commercial Japanese distilled liquors (Shochu) were isolated by headspace solid-phase microexrraction (SPME) and analyzed by gas chromatography (GC) and GC-mass spectrometry (MS). A total of 76 volatile components, including 48 esters, 13 alcohols, and 15 miscellaneous components, were identified. Esters and alcohols constituted the largest groups of quantified volatiles. Differences in volatile components among the distilled liquors and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 77.92% of the total variation across the samples. The samples using barley koji showed higher overall concentrations of total volatile components. Additionally, the principal component analysis did not reveal any sample grouping based on the raw material used.

Influence of Isolation Method on the Composition of Apricot (Prunus armeniaca var. ansu Max.) Flavor (살구의 휘발성 성분 조성에 대한 분리방법의 영향)

  • Kim, Young-Hoi;Kwag, Jai-Jin;Kwon, Young-Ju;Yang, Kwang-Kyu
    • Korean Journal of Food Science and Technology
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    • v.22 no.5
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    • pp.543-548
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    • 1990
  • Volatile components of fresh apricot (Prunus armeniaca var. ansu Max.) were isolated by simultaneous distillation-extraction at two different pH values of 3.1 and 7.0 and by headspace trapping method. The volatiles were analyzed by GC and GC-MS. A total of 80 components were identified in the three aroma concentrates, including 9 naphthalene derivatives that were not previously reported in apricot. Of components identified in native pH (3.1) sample, the major components were aliphatic $C_6$ aldehydes and alcohols, monoterpene alcohols, benzyl alcohol, ${\beta}-phenylethyl$ alcohol and naphthalene derivatives, while those in neutral pH(7.0) sample and headspace volatiles were aliphatic $C_6$ aldehydes and alcohols. Simultaneous distillation-extraction at pH 3.1 was significantly increased the concentration of n-hexanal, trans-2-hexenal, cis-3-hexen-1-ol, linalool oxide, linalool, ${\alpha}-terpineol$, nerol, geraniol, benzyl alcohol, ${\beta}-phenylethyl$ alcohol and naphthalene derivatives. These results demonstrate that above the components are present in glycosidically bound forms in apricot.

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Analysis of Residual Solvents in Food Packaging Materials Using Solid Phase Microextraction Method (Solid Phase Microextraction법을 이용한 식품포장재 중의 잔류용제 분석)

  • 서택교;박상현;이윤수;김정한;권익부
    • Journal of Food Hygiene and Safety
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    • v.14 no.1
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    • pp.76-83
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    • 1999
  • Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

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Composition Studies on the Aromatic Tobacco Varieties (Nicotiana tabacum L. ) : II. Characteristics of Headspace Vapors (향끽미종 잎담배 성분조성에 관한 연구 II. 헤드스페이스 휘발성 유기성분의 특성 조사)

  • Kim, Kyoung-Rae;Lee, Un-chul
    • Journal of the Korean Society of Tobacco Science
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    • v.3 no.1
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    • pp.1-10
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    • 1981
  • Volatile compounds in the headspace vapors of five aromatic tobacco varieties have been examined us ins the polymer adsorption method and high- resolution glass capillary gas chromatography. The gas chromatographic profiles thus obtained were compared, and the aroma composition was found to be characteristic of each tobacco sample with significant differences in the concentrations of major components.

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Comparison of Analytical Methods for Volatile Flavor Compounds in Leaf of Perilla frutescens

  • Kim, Kwan-Su;Ryu, Su-Noh;Song, Ji-Sook;Bang, Jin-Ki;Lee, Bong-Ho
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.44 no.2
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    • pp.154-158
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    • 1999
  • Volatile flavor compounds from perilla leaves were extracted and analyzed with different methods, head-space analysis (HS), simultaneous steam distillation and extraction (SDE) , and solvent extraction (SE), and to compare their efficiencies for quick analysis. Over 30 volatile compounds were isolated and 28 compounds were identified by GC/MSD. Major compound was perillaketone showing the compositions of which were 92% in SDE method, 86% in headspace analysis, and 62% in solvent extraction method. For quick evaluation of leaf flavor in perilla, it was desirable because the headspace analysis method had a shorter analyzing time and smaller sample amount than the other methods.

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The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque (고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법)

  • Ahn Sang-Woo;Lee Si-Jin;Chang Soon-Woong
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.