• Title/Summary/Keyword: headspace GC analysis

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Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Lipase-catalyzed Transeseterification of Corn Oil, Conjugated Linoleic Acid, and Capric Acid in Batch Type Reactor

  • Vu, Phuong-Lan;Shin, Jung-Ah;Lee, Ki-Teak
    • Proceedings of the Korean Society of Postharvest Science and Technology of Agricultural Products Conference
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    • 2003.10a
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    • pp.164.2-165
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    • 2003
  • Structured lipids (SLs) are defined as triacylglycerols to change the fatty acid composition in the glycerol backbone and lipases are known as a powerful tool for the syntheses of SLs. Structured lipid from corn oil, capric acid, and conjugated linoleic acid (CLA) by transesterification reaction and using several amounts of immobilized lipase RM IM (from Rhizomucor miehei) was studied, and 4% of lipase amount was selected for further study as the optimal amount. Comparison the chemical properties (free fatty acid value, iodine value, saponification value, tocopherols, and color analysis), solidification behavior, and volatile fractions (from headspace SPME GC-MS) between com oil and SL com oil was obtained.

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Quantification of Volatile Organic Compounds in Gas Sample Using Headspace Solid-Phase Microextraction (고상 미세 추출법을 이용한 가스시료 중 휘발성유기화합물의 정량 분석)

  • Kim, Jae Hyuck;Kim, Hyunook
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.12
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    • pp.906-917
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    • 2013
  • The purpose of this study is to quantify volatile organic compounds (VOCs) in gas sample using headspace solid-phase microextraction (HS-SPME) coupled to GC analysis. The optimal HS-SPME conditions was CAR/PDMS fiber and 30 min absorprion time for the analysis of various VOCs. In optimal conditions, 80 VOCs could be detected within 1 ppbv and even less than 0.0005 ppbv especially in the case of BTEX. However, fiber reproducibility on adsorption efficiency was 1~9.2% (between the same fiber) and 5.9~13.5% (between the other fiber). We successfully determined 35 VOCs in landfill gas with this method and found that VOCs of high concentration are emitting from vent pipe of closed/open landfill site under the HS-SPME conditions. This method may apply to VOCs/odor determination from various atmospheric environmental samples as well as landfills.

Profiling Patterns of Volatile Organic Compounds in Intact, Senescent, and Litter Red Pine (Pinus densiflora Sieb. et Zucc.) Needles in Winter

  • CHOI, Won-Sil;YANG, Seung-Ok;LEE, Ji-Hyun;CHOI, Eun-Ji;KIM, Yun-Hee;YANG, Jiyoon;PARK, Mi-Jin
    • Journal of the Korean Wood Science and Technology
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    • v.48 no.5
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    • pp.591-607
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    • 2020
  • This study was aimed to investigate the changes of chemical composition of the volatile organic compounds (VOCs) emitted from red pine needles in the process of needle abscission or senescence. The VOCs in intact, senescent, and litter red pine needle samples were analyzed by headspace-solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC/MS). And then, multivariate statistical interpretation of the processed data sets was conducted to investigate similarities and dissimilarities of the needle samples. Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were used to investigate the dataset structure and discrimination between samples, respectively. From the data preview, the levels of major components of VOCs from needles were not significantly different between needle samples. By PCA investigation, the data reduction according to classification based on the chlorophyll a / chlorophyll b (Ca/Cb) ratio were found to be ideal for differentiating intact, senescent, and litter needles. The following OPLS-DA taking Ca/Cb ratio as y-variables showed that needle samples were well grouped on score plot and had the significant discriminant compounds, respectively. Several compounds had significantly correlated with Ca/Cb ratio in a bivariate correlation analysis. Notably, the litter needles had a higher content of oxidized compounds than the intact needles. In summary, we found that chemical compositions of VOCs between intact, senescent, and litter needles are different each other and several compounds reflect characteristic of needle.

Headspace Volatile Compounds of Krill Reaction Flavor and Its Application to Teriyaki Sauce (크릴반응향의 휘발성 향기 성분 및 데리야끼소스의 적용)

  • Kim, Kyoung-Myo;Park, Hyun-Joo;Nam, Min-Hee;Kim, Seong-Bong;Chun, Byung-Soo;Lee, Yang-Bong
    • Culinary science and hospitality research
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    • v.19 no.3
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    • pp.105-115
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    • 2013
  • Maillard reaction flavors had been tried by using krill hydrolysate and precursors in order to develop Teriyaki sauce with the reaction flavors. Also, the study for applying krill to Teriyaki sauce had been tried by using krill instead of eel bones. To make boiled-type and grilled-type reaction flavors, krill hydrolysate was used with other precursors such as serine, glucose and glucosamine. In the dynamic analysis of headspace volatile compounds, 20 mL reaction flavor was analyzed by the combined system of purge & trap, automatic desorber, gas chromatography and mass selective detector. Three kinds of Teriyaki sauce were developed with reaction flavor, krill and eel bones, and their products were evaluated by 10 items of cooked vegetables, cooked potatoes, boiled shrimp, grilled shrimp, fishy smell, pungent aroma, burned smell, sweety aroma, chemical smell, mud smell and preference. In the results of headspace analysis, 35 and 33 volatile compounds were identified from grilled-type and boiled-type reaction flavors. Grilled-type had sulfur-containing, aliphatic compounds, alcohols, ketones, pyrazines, and other aromatic compounds, and grilled-type had aldehydes, furans, other nitrogen-containing compounds. In the sensory evaluation of Teriyaki sauce, the items of roasted shrimp and sweety aroma showed significant differences for grilled-type application to Teriyaki sauce. The above results show the possible application of grilled-type reaction flavor to Teriyaki sauce.

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Effects of High Hydrostatic Pressure and pH on the Reduction of Garlic Off-flavor (초고압처리 시간과 pH 변화에 의한 마늘의 이취성분 저감화)

  • Lim, Chae-Lan;Hong, Eun-Jeung;Noh, Bong-Soo;Choi, Won-Seok
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.533-540
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    • 2010
  • Effects of pH (1.8-10.2) and time (56 sec-15 min 4 sec) at high hydrostatic pressure (500 MPa) on the reduction of volatile compounds in garlic were studied. Volatile components of garlic were obtained from the headspace, analyzed, and identified by gas chromatography (GC)-mass spectrometry and an electronic nose. Nineteen sulfur compounds were identified as major compounds in garlic, and furan, aldehydes, alcohols, and ketones were also detected. Off-flavor compounds were more effectively reduced under strong acidic conditions. As the residence time at 500 MPa increased from 56 sec to 15 min 4 sec, the total amount of volatile compounds decreased significantly. The total amount of sulfur compounds decreased about 70% compared to those of raw garlic when the garlic was soaked in buffer (pH 6.0) and treated at 500 MPa for 15 min 4 sec. A principal component analysis showed that the off-flavors of garlic were reduced by the operating time of high hydrostatic pressure as well as pH treatment. The correlation coefficient of the results between GC and the electronic nose analysis was 0.9620. Therefore, pH and high hydrostatic pressure treatment could be used as an efficient method for reducing of garlic off-flavor.

Changes in aroma compounds of decaffeinated coffee beans (디카페인 커피 원두의 향기성분 변화)

  • Jin-Young Lee;Young-Soo Kim
    • Food Science and Preservation
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    • v.30 no.3
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    • pp.492-501
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    • 2023
  • In this study, we wanted to understand the impact of different decaffeination processes on aroma compounds of coffee. Therefore, we analyzed differences in physical characteristics and volatile aroma compounds profiles of regular coffee (RC), Swiss water process decaffeinated coffee (SWDC), and supercritical CO2 decaffeinated coffee (SCDC) after roasting the coffee beans. The electronic nose analysis identified RC and SCDC as different groups which indicates that these groups volatile aroma compound compositions were different. The principal component analysis of volatile compound patterns identified using an electronic nose indicated that there was a large difference in volatile compounds between RC, which was not decaffeinated, and both decaffeinated SWDC and SCDC. The major aroma compounds of RC, SWDC and SCDC were propan-2-one and hexan-2-one which are ketone, and hexanal and (E)-2-pentenal which are aldehyde and 3-methyl-1-butanol which is an alcohol. After roasting, the composition of major volatile compounds appearing in the beans was similar, but the relative odor intensity was different. We identified 28 volatile aroma compounds from RC, SWDC, and SCDC using headspace-solid phase microextraction-gas chromatography/mass spectrometry (HS-SPME-GC/MS), and analyzed 10 major compounds that were present in high abundance, including furfural, 2-furanmethanol, 2,5-dimethylpyrazine, and 2-ethyl-3-methylpyrazine.

Development of the testing method for vinyl chloride monomer (VCM) in polyvinyl chloride(PVC) samples (PVC 제품에서의 염화비닐 단량체 정량분석 방법에 관한 연구)

  • Kweon, Deok-Jun;Choi, Ki-In;Eom, Hui-Jeong;Lee, Jae-In;Choi, Zel-Ho
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.395-401
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    • 2012
  • This study presents a method for the quantitative analysis of residual vinyl chloride monomer (VCM) in PVC products. In elution solvent, the extraction efficiency was similar by ethanol, THF, and acetone, but using n-hexane, it indicated relatively low extraction efficiency. Measuring VCM in the pulverized PVC samples, it showed reasonable results in both the direct injection method and headspace method with GC/MS. Regarding analysis of VCM in the intermediate sponge samples, five laboratories showed good results, and from the results, it was considered that VCM quantitative method in this study was reliable.

Aroma Profiling of Sun-dried Salt by GC/MS Analysis (GS/MS 분석에 의한 천일염의 향기성분)

  • Na, Jong Min;Jin, Yong Xie;Kim, Se Na;Kim, Jung Bong;Kim, Haeng Ran;Cho, Young Suk;Yoon, Hyang Sik;Kim, So-Youn
    • The Korean Journal of Food And Nutrition
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    • v.25 no.4
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    • pp.1092-1098
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    • 2012
  • Aroma compounds in sun-dried salt according to saltern material and packaging box were extracted by the headspace and were isolated by using GC-MS. These compounds were identified including ketones, heterocyclic compounds and six other compounds. Major aroma compounds in salts were identified as 4-methyl-2-pentanone, 5-methyl-3-hexanone, 4-methyl-3-penten-2-one, 2-hexanol, benzothiazole, 2,4-bis(1,1-dimethylethyl)-phenol, and 1,3,5-tri-tert-butyl benzene. However, we found no significant differences according to the saltern materials in three salts. Salts stored in Chamaceyparis obtusa (Sieb. et Zucc.) had more diverse aroma profiling than those in Pinus densiflora and Paulownia coreana. We consider that it need to research the development of high value added products for new aromatic salt.

Analysis of Volatile Organic Compounds in Sediments Using HS-GC/MS - Confirmation of Matrix Effects in External and Internal Standard Methods - (HS-GC/MS를 이용한 퇴적물 중 휘발성유기화합물 분석 - 외부 및 내부표준방법에서 매질영향 확인 -)

  • Shin, Myoung-Chul;Jung, Da-som;Noh, Hye-ran;Yu, Soon-ju;Seo, Yong-Chan;Lee, Bo-Mi
    • Journal of Korean Society on Water Environment
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    • v.37 no.6
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    • pp.510-519
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    • 2021
  • Volatile Organic Compounds (VOCs) in sediments, which can cause human health problems, have been monitored in Korea since 2014. Measured VOC concentrations can be affected by matrix type and the volatility of target substances. In this study, (1) VOCs volatility and the influence of matrix interference were confirmed, and (2) internal standards (IS) method was applied to improve analytical method. For these purposes, method detection limit (MDL), calibration linearity, precision and accuracy of VOCs were compared in various matrices using the IS. Some of VOCs in sediments showed different peak areas and reduced rates compared to water matrix. It was suggested that adsorption properties of sediments hindered the migration to vapor during heat pretreatment in headspace method. A calibration curve was created in clean sand. Recovery rates for the calibration curve method and IS applying method were 64.1~83.1% and 99.1~119.3%, respectively. Relative standard deviations ranged from 11.1% to 21.6% for the calibration curve method and those for IS ranged 4.7% to 13.7%. In case of real sediment, calibration curve and 1,2-Dichlorobenzene-d4 (ODCB) among IS were not suitable. The average recovery rate of Fluorobenzene (FBZ) increased by 56.4% and Relative Standard Deviation (RSD) by 4.7%. However, the recovery rate was increased in the samples with large values of igniting intensity. This study confirmed that influence of the matrix of VOCs in sediment, and addition of IS materials improved precision and accuracy. Although IS corrects volatilization and adsorption, it is recommended that more than two types of IS should be added rather than single.