• Title/Summary/Keyword: solid-phase microextraction/gas chromatography mass spectrometry

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Analysis of Residual Furan in Human Blood Using Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (SPME-GC/MS)

  • Lee, Yun-Kyung;Jung, Seung-Won;Lee, Sung-Joon;Lee, Kwang-Geun
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.379-383
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    • 2009
  • For an accurate risk assessment of furan, a potential human carcinogen, levels must be determined in human blood plasma using a simple and robust assay. In this study, solid phase microextraction-gas chromatography/mass spectrometry (SPME-GC/MS) was used to analyze blood plasma levels of furan in 100 healthy individuals who consumed a normal diet. The subjects were 30 to 70 years of age and 51% were women. Ultimately, an analytical method was established for analyzing furan in human blood. The limit of quantification (LOQ) and furan recovery rate in blood were 1.0 ppb and 104%, respectively. Finally, furan was detected in 21 individuals (13 males, 8 females) with levels ranging up to 17.86 ppb (ng furan/g food).

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.

Headspace-Solid Phase Microextraction (HS-SPME) Analysis of Korean Fermented Soybean Pastes

  • Lee, Seung-Joo
    • Food Science and Biotechnology
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    • v.18 no.3
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    • pp.700-705
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    • 2009
  • In this study, the volatile compounds in 9 commercial fermented soybean pastes were extracted and analyzed by headspace-solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), respectively. A total of 63 volatile components, including 21 esters, 7 alcohols, 7 acids, 8 pyrazines, 5 volatile phenols, 3 ketones, 6 aldehydes, and 6 miscellaneous compounds, were identified. Esters, acids, and pyrazines were the largest groups among the quantified volatiles. About 50% of the total quantified volatile material was contributed by 5 compounds in 9 soybean paste samples; ethyl hexadecanoate, acetic acid, butanoic acid, 2/3-methyl butanoic acid, and tetramethyl-pyrazine. Three samples (CJW, SIN, and HAE) made by Aspergillus oryzae inoculation showed similar volatile patterns as shown in principal component analyses to GC-MS data sets, which showed higher levels in ethyl esters and 2-methoxy-4-vinylphenol. Traditional fermented soybean pastes showed overall higher levels in pyrazines and acids contents.

Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

  • Jung, Mi-Jin;Shin, Yeon-Jae;Oh, Se-Yeon;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.27 no.2
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    • pp.231-236
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    • 2006
  • A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

Effect of Stewing Time on the Small Molecular Metabolites, Free Fatty Acids, and Volatile Flavor Compounds in Chicken Broth

  • Rong Jia;Yucai Yang;Guozhou Liao;Yuan Yang;Dahai Gu;Guiying Wang
    • Food Science of Animal Resources
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    • v.44 no.3
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    • pp.651-661
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    • 2024
  • Chicken broth has a taste of umami, and the stewing time has an important effect on the quality of chicken broth, but there are fewer studies on the control of the stewing time. Based on this, the study was conducted to analyze the effects of different stewing times on the sensory, small molecular metabolites, free fatty acids, and volatile flavor compounds contents in chicken broths by liquid chromatography-quadrupole/time-of-flight mass spectrometry, gas chromatography-mass spectrometry, headspace solid-phase microextraction, and gas chromatography-mass spectrometry. Eighty-nine small molecular metabolites, 15 free fatty acids, and 86 volatile flavor compounds were detected. Palmitic and stearic acids were the more abundant fatty acids, and aldehydes were the main volatile flavor compounds. The study found that chicken broth had the best sensory evaluation, the highest content of taste components, and the richest content of volatile flavor components when the stewing time was 2.5 h. This study investigated the effect of stewing time on the quality of chicken broth to provide scientific and theoretical guidance for developing and utilizing local chicken.

Volatile Metabolic Markers for Monitoring Pectobacterium carotovorum subsp. carotovorum Using Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

  • Yang, Ji-Su;Lee, Hae-Won;Song, Hyeyeon;Ha, Ji-Hyoung
    • Journal of Microbiology and Biotechnology
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    • v.31 no.1
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    • pp.70-78
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    • 2021
  • Identifying the extracellular metabolites of microorganisms in fresh vegetables is industrially useful for assessing the quality of processed foods. Pectobacterium carotovorum subsp. carotovorum (PCC) is a plant pathogenic bacterium that causes soft rot disease in cabbages. This microbial species in plant tissues can emit specific volatile molecules with odors that are characteristic of the host cell tissues and PCC species. In this study, we used headspace solid-phase microextraction followed by gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS) to identify volatile compounds (VCs) in PCC-inoculated cabbage at different storage temperatures. HS-SPME-GC-MS allowed for recognition of extracellular metabolites in PCC-infected cabbages by identifying specific volatile metabolic markers. We identified 4-ethyl-5-methylthiazole and 3-butenyl isothiocyanate as markers of fresh cabbages, whereas 2,3-butanediol and ethyl acetate were identified as markers of soft rot in PCC-infected cabbages. These analytical results demonstrate a suitable approach for establishing non-destructive plant pathogen-diagnosis techniques as alternatives to standard methods, within the framework of developing rapid and efficient analytical techniques for monitoring plant-borne bacterial pathogens. Moreover, our techniques could have promising applications in managing the freshness and quality control of cabbages.

Identification the Key Odorants in Different Parts of Hyla Rabbit Meat via Solid Phase Microextraction Using Gas Chromatography Mass Spectrometry

  • Xie, Yuejie;He, Zhifei;Lv, Jingzhi;Zhang, En;Li, Hongjun
    • Food Science of Animal Resources
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    • v.36 no.6
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    • pp.719-728
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    • 2016
  • The aim of this study was to explore the volatile compounds of hind leg, foreleg, abdomen and Longissimus dorsi in both male and female Hyla rabbit meat by solid phase microextraction tandem with gas chromatography mass spectrometry, and to seek out the key odorants via calculating the odor activity value and principal component analysis. Cluster analysis is used to study the flavor pattern differences in four edible parts. Sixty three volatile compounds were detected, including 23 aldehydes, 4 alcohols, 5 ketones, 11 esters, 5 aromatics, 8 acids and 7 hydrocarbons. Among them, 6 aldehydes and 3 acids were identified as the potential key odorants according to the ratio of concentration and threshold. The contents of volatile compounds in male Hyla rabbit meat were significantly higher than those in female one (p<0.05). The results of principal component analysis showed that the first two principal component cumulative variance contributions reach 87.69%; Hexanal, octanal, 2-nonenal, 2-decenal and decanal were regard as the key odorants of Hyla rabbit meat by combining odor activity value and principal component analysis. Therefore volatile compounds of rabbit meat can be effectively characterized. Cluster analysis indicated that volatile chemical compounds of Longissimus dorsi were significantly different from other three parts, which provide reliable information for rabbit processing industry and for possible future sale.

Determination of Volatile Organic Compounds (VOCs) in Drinking Water using Solid Phase Microextraction (SPME) (SPME를 이용한 수용액중의 휘발성 유기화합물 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.277-281
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    • 2000
  • The solid phase microextrction (SPME) fiber which contains $100{\mu}m$ polydimethyl siloxane of a stationary phase was used for the analysis of volatile organic compounds contained in aqueous solution. sixteen volatile organic compounds, which were spiked in blank water and extracted by the headspace SPME techique, were analyzed by gas chromatography/mass spectrometry (GC/MS). Analytical results showed that the percent of average recoveries and relative standard deviations were 97% and 4.7%, respectively. The value of detection limit was ranged from 0.01 to $0.5{\mu}g/l$. These results are more accurate than those obtained by the other methods such as purge and trap and headspace methods.

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Extraction Methods of Organic Components from Rubber Composites and Analysis of the Extract Using Gas Chromatography/Mass Spectrometry

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.54 no.3
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    • pp.188-200
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    • 2019
  • Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.