• Title/Summary/Keyword: GC-SPME

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Aroma Characteristic of Chungkukjang with Astragalus membranaceus (황기청국장의 향기특성)

  • Yoon Hyang-Sik;Choi Hye-Sun;Joo Seon-Jong;Kim Ki-Sik;Kim Sook-Jeong
    • Food Science and Preservation
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    • v.13 no.2
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    • pp.269-272
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    • 2006
  • Aroma compounds in chungkukjang with Astragalus membranaceus (Hwangki) were extracted by the simultaneous distillation and extraction (SDE), headspace and solid phase microextraction (SPME), and aroma compounds obtained by this method were identified with GC-MS. Thirty compounds were identified, including six ketones, eight alcohols, three heterocyclic compounds, three aldehydes, five hydrocarbones and five other compounds. Major aroma compounds were identified as 3-hydroxy-2-butanone, 2-furanmethanol, 2-methoxy-4-vinylphenol, and 4-vinylphenol in SDE, 2,3-butanedione, 3-hydroxy-2-butanone, ethanol, 2,6-dimethyl pyrazine and acetic acid in headspace and acetone, ethanol, 2,5-dimethyl pyrazine, tetramethyl pyrazine and acetic acid in SPME. The content of pyrazines identified in headspace and SPME methods was higher than that of SDE method, and the content of pyrazines containing 2,5-dimethyl pyrazine, 2,6-dimethyl pyrazine and tetramethyl pyrazine in chungkukjang was higher than that of Hwangki chungkukjang.

Study of the Presence of Residual Hexane in Olive Oils (유통 올리브유의 잔류 헥산에 대한 연구)

  • Kim, Nam-Sook;Lee, Jeung-Hee;Heo, Ok-Soon;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.10
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    • pp.1405-1411
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    • 2006
  • The presence and content of residual hexane in the olive oils were studied. Total 41 olive oils of imported and domestic brands, which were labeled as extra virgin and refined (mixed), were collected from the market. For analysis, electronic nose and headspace SPME-GC/MS were used. Electronic nose equipped with 12 metal oxide sensors was used for the discrimination of odor pattern of olive oils against the different concentrations of hexane. From the results, it is assumed that the contents of residual hexane in the collected olive oils were below 5 ppm. For Qualitative and quantitative analysis of hexane, polydimethylsiloxane (PDMS) fiber was employed for SPME-GC/MS. In the results, the peak of residual hexane was detected in 8 samples from 41 olive oils. But the detected level was no more than 1 ppm that is under the regulation limit (5 ppm) by Korea Food Additive Code.

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.

Determination of Plasticizers included in Balloon by Solid Phase Microextraction and Gas Chromatography with Mass Spectrometric Detection (SPME-GC-MS를 이용하여 풍선에 포함된 가소제의 분석)

  • Park, Hyun-Mee;Kim, Ji-Hyun;Ryu, Jae-Chun;Kim, Young-Man;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.44-49
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    • 2001
  • Solid-phase microextraction (SPME) with $85{\mu}m$ polyacrylate fiber, coupled to gas chromatography-mass spectrometry was used to analyze the plasticizers contained in balloon samples. The balloons were identified to be made of polyisoprene by IR spectroscopy. The plasticizers extracted from the balloon samples soaked in acetone-added water solvent for an hour were quantified by external standard method using nine kinds of plasticizers. The quantification method was validated for standard plasticizers in the range of $0.25-25{\mu}g/g$. The detection limits were $0.11-0.38{\mu}g/g$ for different plasticizers. The RSDs for the reproducibility of this quantitation method were 3.7-14.2%. A few of balloons included risky level of plasticizer concerned as and endocrine disrupter, and it is necessary to regulate these products.

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Analysis of Volatile Fatty Acids in Air by Dynamic SPME (Dynamic SPME를 이용한 공기 중 지방산 분석)

  • Yu, Mee-Seon;Yang, Sung-Bong;Ha, Nam-Ki
    • Journal of Environmental Science International
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    • v.19 no.12
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    • pp.1447-1454
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    • 2010
  • In this study, the detection limits of lower fatty acids in air were investigated by using Dynamic SPME(Solid Phase Micro-Extraction), i.e. improved Head Space - SPME method(HS-SPME). This Dynamic SPME, called SPDE(Solid Phase Dynamic Extraction), is the analytical method for volatile compounds in air with the extraction by using a stainless steel needle of which inner surface is coated with adsorption material and following the gas chromatographic analysis by inserting the needle into a injection port of GC and subsequently, desorption of the volatile compounds into a gas-chromatographic column. Extraction was carried out by passing the sample air through the needle with a suction pump which has been used for a detection tube. The result of measurement for the 6 lower fatty acids showed that the detection limits ranged from 0.10 ppm to 0.44 ppm and the linear correlation coefficients were over 0.99. Relative standard deviations obtained from 5 analytical repetition of a ca. 1.6 ppm standard mixture were in the range of 1.87%~2.47%. This method has been shown to be a adequate for the measuring C2~C5 fatty acids in air in the concentrations of over several hundreds ppb.

Determination of VOC in aqueous samples by the combination of headspace (HS) and solid-phase microextraction (SPME) (HS-SPME 방식에 기초한 물 중 VOC 성분의 분석기법에 대한 연구: 3가지 실험 조건의 변화와 분석감도의 관계)

  • Park, Shin-Young;Kim, Ki-Hyun;Yang, H.S.;Ha, Joo-Young;Lee, Ki-Han;Ahn, Ji-Won
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.93-101
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    • 2008
  • The application of solid phase microextraction (SPME) is generally conducted by directly immersing the fiber into the liquid sample or by exposing the fiber in the head space (HS). The extraction temperature, the time of incubation, and application of stirring are often designated to be the most important parameters for achieving the best extraction efficiencies of HS-SPME analysis. In this study, relative importance of these three analytical parameters involved in the HS-SPME method is evaluated using a polydimethylsiloxane/carboxen (PDMS/CAR) fiber. To optimize its operation conditions the competing relationships between different parameters were investigated by comparing the extraction efficiency based on the combination of three parameters and two contracting conditions: (1) heating the sample at 30 vs. 50 C, (2) exposing samples at two durations of 10 vs. 30 min, and (3) application of stirring vs. no stirring. According to our analysis among 8 combination types of HS-SPME method, an extraction condition termed as S50-30 condition ((1) 1200 rpm stirring, (2) $50^{\circ}C$ exposure temp, and (3) 30 min exposure duration) showed maximum recovery rate of 45.5~68.5% relative to an arbitrary reference of direct GC injection. According to this study, the employment of stirring is the most crucial factor to improve extraction efficiency in the application of HS-SPME.

Volatile Component of Pine Needles from Pinus densiflora S. using Solid Phase Microextraction-Ges Chromatography-Mass Spectrometry

  • Lee Jae-Gon;Lee Chang-Gook;Back Shin;Jang Hee-Jin;Kwag Jae-Jin;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.18 no.4
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    • pp.373-379
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    • 2005
  • The volatile components of Pinus densiflora needles were studied by gas chromatography-mass spectrometry(GC-MS), using seven kinds of solid phase microextraction (SPME) fibers, seven in SPME fibers: 100 ${\mu}m$ PDMS, 65 ${\mu}m$ PDMS/DVB, 65 ${\mu}m$ SF-PDMS/DVB, 85 ${\mu}m$ PA, 75 ${\mu}m$ CAR/PDMS, 65 ${\mu}m$ CW/DVB and 50/30 ${\mu}m$ DVB/CAR/PDMS fibers. A total of 40 components were identified by using the seven different SPME fibers. The identified components were classified, according to their functionalities, as follows: 26 hydro-carbons, 7 alcohols, 4 carbonyl compounds, and 3 esters. The major volatile components of Pinus densiflora needles identified by these SPME fibers were $\alpha$-pinene ($1.7\~21.7\;{\mu}g/g$), $\beta$-myrcene ($2.0\~20.1\;{\mu}g/g$), $\beta$-phel-landrene ($4.6\~22.8\;{\mu}g/g$), $\beta$-caryophyllene ($6.7\~26.0\;{\mu}g/g$) germacrene D ($1.1\~11.9\;{\mu}g/g$). In the comparison of the seven SPME fibers, PDMS appeared to be the most suitable fiber for the analysis of hydrocarbon compounds and CAR/DPMS, PDMS/DVB, CW/VB and DVB/CAR/PDMS are shown to be optimal for analysis of the alcohols and carbonyl compounds.

Optimization Study of Trace Analysis of Potential Diesel Oxygenate Using the Design Of Experiment (DOE) in Solid-Phase Microextraction with GC/FID (고체상미량분석법(SPME-GC/FID)에서 실험계획법을 이용한 디젤첨가제 미량분석의 최적화 연구)

  • Park, Jae-Sang;Chang, Soon-Woong
    • Journal of Soil and Groundwater Environment
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    • v.12 no.5
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    • pp.73-85
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    • 2007
  • In this study, the experiment of solid-phase microextraction (SPME) technique using GC/FID was conducted as a possible alternative to liquid-liquid extraction for the analysis of EGBE, DGBE, DBM and TGME in water, and also, an optimization condition of trace analysis for disel oxygenates including EGBE by the design of experiment (DOE) was described. Experiments used a fractional factorial design method followed by central composite design allowing optimization of a number of factors as well as statistical analysis of the results. The response surface analysis showed that the extraction efficiency could be represented by a second-order polynomial equation in which the salts concentration, extraction temperature, extraction time and sonication time are the major influences. Using DOE method, a new datadependent method was developed to improve the quantity of confidently analyzed disel oxygenates in water samples.

Thermal Changes of Aroma Components in Soybean Pastes (Doenjang) (된장 가열조리 시 생성되는 향기성분 변화)

  • Lee, Seung-Joo;Ahn, Bo-Mi
    • Korean Journal of Food Science and Technology
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    • v.40 no.3
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    • pp.271-276
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    • 2008
  • In this study, volatile compounds were isolated from traditional and commercial fermented soybean pastes according to different heating temperatures (room temperature, $50^{\circ}C$, $100^{\circ}C$) using headspace-solid phase microextraction (HS-SPME). The compounds were then analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 51 volatile components, including 18 esters, 3 alcohols, 6 acids, 8 pyrazines, 5 volatile phenols, 6 aldehydes, and 5 miscellaneous compounds, were identified. Esters and acids such as ethyl hexadecanoate, acetic acid, and 2/3-methyl butanoic acid were the largest groups among the quantified volatiles. By applying principal component analyses to the GCMS data sets, differences were observed in the volatile components of the soybean pastes as to the different heating temperatures. A large variation was shown between the volatile components of the traditional and commercial soybean pastes by increasing the heating temperature. Commercial samples had significantly higher levels of longer chain ethyl esters, aldehydes, and thermal degradation products such as maltol and 2-acetyl pyrrole, while traditional samples showed higher concentrations of acids and pyrazines.

Identification of Volatile Compounds of 4 Grape Species by Storage Conditions (전자코와 GC/MS를 이용한 포도 품종별 저장 조건에 따른 휘발성 향기 성분 연구)

  • Lee, Yun-Jeung;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.7
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    • pp.874-880
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    • 2007
  • Volatile flavor compounds of 4 grape species (Campbell, Sheridan, Red globe, and Meoru) were identified during 3-day storage at either $4^{\circ}C$ or room temperature. Each sample was analyzed by solid-phase micro-extraction (SPME) method combined with gas chromatography-mass spectrometry. Also electronic nose composed of 12 different metal oxide sensors was used to differentiate flavors of grapes. Sensitivities (delta $R_{gas}/R_{air}$) of sensors from electronic nose were obtained by principal component analysis (PCA). Proportion of the first principal component was 99.30% at $4^{\circ}C$ and 99.36% at room temperature, respectively. In our result, flavor patterns of grape can be differentiated according to the storage period. The major volatile flavor compounds were 1-hexanol, hexanoic acid and its ethyl ester, and phenylethyl alcohol with the presence of butanoic acid and its ethyl ester, acetic acid, benzeneacetic acid and its ethyl ester.