• Title/Summary/Keyword: headspace sample

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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.

Removal of residual VOCs in a collection chamber using decompression for analysis of large volatile sample

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.23-35
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    • 2021
  • In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

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
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    • v.51 no.3
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    • pp.238-244
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    • 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.

Analytical Method of Epichlorohydrin in Canned Beverages by Purge-and- Trap/GC

  • Lee Kwang-Ho;Kwak In-Shin;Kim Dyoung-Il;Choi Byoung-Hee;Kim Guy-Joung;Lee Chul-Won
    • Proceedings of the Korean Society of Food Hygiene and Safety Conference
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    • 2001.10a
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    • pp.140-140
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    • 2001
  • A sensitive analytical method based on gas chromatograpy-mass spectrometry with a selected ion monitoring (GC/MS-SIM) with the purge-and-trap concentration and with headspace method (in limited applications) was developed for determining of epichlorohydrin in canned beverages coated with epoxy resin. The calibration curve in the range of $0.5\sim50ng$ had correlation coefficient greater than 0.998 and a detection limit of $0.l\mug/L$ was obtained using a sample volume of 20ml. The predominant ions of epichlorohydrin produced in MSD using electron ionization(EI) were m/z 57 ([M-CI]+) and 62/64 $([M-CH_2O]+)$. In survey of epichlorohydrin in thirty commercial canned beverage samples, none of them was detected.

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Poly(dimethylsiloxane) Mini-disk Extraction

  • Cha, Eun-Ju;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3603-3609
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    • 2011
  • A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

Volatile Compounds for Discrimination between Beef, Pork, and Their Admixture Using Solid-Phase-Microextraction-Gas Chromatography-Mass Spectrometry (SPME-GC-MS) and Chemometrics Analysis

  • Zubayed Ahamed;Jin-Kyu Seo;Jeong-Uk Eom;Han-Sul Yang
    • Food Science of Animal Resources
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    • v.44 no.4
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    • pp.934-950
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    • 2024
  • This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

Mornitoring of 1-hexene and 1-octene in Hygienic Polyethylene-based Packaging (폴리에틸렌계 위생용 용기포장재중의 1-hexen과 1-octene 조사)

  • Cho, Sung-Ja;Kim, Ae-Kyung;Kwak, Jae-Eun;Kim, Ji-Young;Kim, Si-Jung;Kum, Jin-Young;Kim, Il-Young;Kim, Jung-Hun;Chae, Young-Zoo
    • Journal of Food Hygiene and Safety
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    • v.26 no.4
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    • pp.383-387
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    • 2011
  • The levels of migration of 1-hexene and 1-octene residues in PE (polyethylene) products were analyzed by Headspace gaschromatography (HSGC). A total of 21 samples were including lap, polyglove, zipper bag and ect. The samples were eluted with distilled water, 4% acetic acid, 20% ethanol and n-heptan. The limit of detection (LOD) was 0.06 mg/L ~ 0.30 mg/L and limit of quantitation (LOQ) was 0.21 mg/L ~ 1.01 mg/L, respectively. But because of the high volatile, n-heptan elution was not detected 1-hexene and 1-octene standard. 1-hexene and 1-octene were not detected in the sample which eluted with simulant at $60^{\circ}C$, 30min. Microwave for 1 minute also treated sample and direct heated at $100^{\circ}C$ without simulant were not detected.

Estimation of Methanol Exposure Level via Alcoholic Beverage Consumed by Jecheon Citizen, South Korea (주류 섭취로 인한 대한민국 제천 시민의 메탄올 노출수준 평가)

  • Oh, Chang-Hwan;Lee, Ye-Ji;Min, Sung Hee
    • The Korean Journal of Food And Nutrition
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    • v.26 no.1
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    • pp.44-50
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    • 2013
  • Quantitative analyses of naturally occurring methanol were performed for the alcoholic beverages commonly consumed in Jecheon, Chungbuk province, South Korea. The headspace analysis method was optimized for the low and high alcoholic beverages. The external standard method was applied due to the overlapping of 2-propanol and 2-butanol (the internal standard candidates) with target sample matrix peaks. The target samples were selected based on the retail sales amounts of alcoholic beverages in the largest retailer food-mart chain, Jecheon, Chungbuk province, South Korea. There was no sample containing methanol over 0.5 $mg/m{\ell}$, the Korean maximum level of methanol in alcoholic beverages (1.0 $mg/m{\ell}$ for fruit originated liquor etc). The total exposure amount of methanol via alcoholic beverages was estimated based on the daily alcohol consumption of 40 g. The hazard indices calculated by methanol RfD 0.5 mg/kg bw day (US EPA) and ADI 20 mg/kg bw day (proposed by Lachenmeier etc.) were 0.301 and 0.008, respectively. As with the hazard index, aggregate exposures below a HI of 1.0 will likely not result in adverse noncancer health effects over a lifetime of exposure. Then the methanol exposure via the alcoholic liquours might not hazard to Jecheon citizen.

Adsorption and Removal of Volatile Organic Compounds from Fabrics with β-Cyclodextrin Finish (직물의 β-cyclodextrin 가공에 따른 휘발성 유기성분의 흡착과 제거)

  • Chung, Haewon;Hwang, Nawon;Kim, Joo-Yeon;Shin, Seung-Yeop
    • Journal of the Korean Society of Clothing and Textiles
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    • v.37 no.1
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    • pp.113-123
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    • 2013
  • Clothes that retain and emanate body odor feel uncomfortable and unclean; subsequently, the adsorption, desorption and removal amounts of malodorous compounds from fabrics with different polarities were examined. 1-Octen-3-one, octanal and isovaleric acid, which are important malodor compounds from the body, were used as volatile organic compounds (VOC). Samples were prepared with unfinished and ${\beta}$-CD finished cotton, nylon and PET fabrics. The amounts of VOCs retained on the fabrics were measured using headspace GC-MS; in addition, the odor intensity of the samples were evaluated by 10 trained panelists. The amounts adsorbed were estimated by weight gain; however, moisture was found to have a larger effect on the increase in weight than VOCs. The polarity of the VOCs decreased in the order of isovaleric acid, octanal and 1-octen-3-one. Despite the exceptionally large amounts of octanal adsorbed on the nylon sample, the amounts of malodorous compounds adsorbed on fabrics increased with the decreasing VOC molecular weight. The unfinished PET sample adsorbed more VOCs than the unfinished-fabric samples. The odor intensity was mostly weaker in the ${\beta}$-CD finished fabrics than in the unfinished fabrics. The odor intensity of the ${\beta}$-CD finished fabrics was lower than unfinished fabrics. The amount of VOCs that remained on the soiled fabric samples after storing in air for 24 hrs decreased with the increasing VOC vapor pressure. Most VOCs were removed by washing; however, more VOCs were left on the ${\beta}$-CD finished fabrics than unfinished fabrics. The intensity of the odor from the unfinished PET and ${\beta}$-CD finished fabrics was stronger and weaker, respectively, than that of other fabrics, even when the same amounts of VOCs remained.

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.