• Title/Summary/Keyword: GC-SPME

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Separation and recovery of semi-volatile substances of Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus by reduced pressure collections and GC-MS

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.11-22
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    • 2020
  • When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

Studies on the Free and Bound Aroma Compounds in Green and Fermented Teas (녹차와 후발효차의 유리형 및 결합형 향기성분에 대한 연구)

  • Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.43 no.4
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    • pp.407-412
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    • 2011
  • Free and bound aroma compounds in green and fermented teas treated with microbial-fermentation were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. Aldehydes and ketones in green tea decreased during microbial fermentation, whereas linalool and geraniol increased in the fermented tea. After enzyme treatment, (Z)-3-hexen-1-ol increased significantly following enzymatic hydrolysis of both green and fermented teas. In addition, benzaldehyde, 3-hexenyl acetate, and geraniol also increased in green tea with enzyme treatment. Bound aroma compounds in the green and fermented teas increased at different levels of added enzyme. We demonstrated the enhancement of both green and fermented teas by enzyme treatment, which can lead to improvement in the flavor qualities of green and fermented teas.

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.

The Global Volatile Signature of Veal via Solid-phase Microextraction and Gas Chromatography-mass Spectrometry

  • Wei, Jinmei;Wan, Kun;Luo, Yuzhu;Zhang, Li
    • Food Science of Animal Resources
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    • v.34 no.5
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    • pp.700-708
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    • 2014
  • The volatile composition of veal has yet to be reported and is one of the important factors determining meat character and quality. To identify the most important aroma compounds in veal from Holstein bull calves fed one of three diets, samples were subjected to solid-phase microextraction (SPME) combined with gas chromatography-quadrupole mass spectrometry (GC-MS). Most of the important odorants were aldehydes and alcohols. For group A (veal calves fed entirely on milk for 90 d before slaughter), the most abundant compound class was the aldehydes (52.231%), while that was alcohols (26.260%) in group C (veal calves fed starter diet for at least 60 d before slaughter). In both classes the absolute percentages of the volatile compounds in veal were different indicating that the veal diet significantly (p<0.05) affected headspace volatile composition in veal as determined by principal component analysis (PCA). Twenty three volatile compounds showed significance by using a partial least-squared discriminate analysis (PLS-DA) (VIP>1). The establishment of the global volatile signature of veal may be a useful tool to define the beef diet that improves the organoleptic characteristics of the meat and consequently impacts both its taste and economic value.

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.

Volatile Flavor Compounds Derived from Anchovy Engraulis japonicus Sauce Residues through Maillard Reactions (멸치(Engraulis japonicus) 액젓 부산물로부터 마이야르 반응을 통해 유도 된 휘발성 향기성분)

  • Jin Hyeon Kim;Yong-Jun Cha;Daeung Yu
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.56 no.2
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    • pp.174-181
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    • 2023
  • Volatile flavor compounds of optimal Maillard reactions (MR) derived with the addition of precursors (AP), control (without AP) and raw as anchovy Engraulis japonicus sauce residue were identified and comparatively analyzed using solid phase microextraction/gas chromatography/mass spectrometry (SPME/GC/MS). MR was produced by adding 1% (w/w) glucose and mixed amino acids (threonine 0.543%, glutamic acid 0.194%, glycine 0.382%, w/w) to raw (100 g of anchovy sauce residue and 100 mL of distilled water), and heating at 110 ℃ for 2 h. Among 65 flavor components detected, 7 compounds were produced through Maillard reaction to change in content. A total of 7 volatile flavor compounds, including 2-methylbutanal, 3-methylbutanal, dimethyl disulfide, methylpyrazine, dimethyl trisulfide, methional, and 2-furanmethanol, tended to increase in the order of raw, control, and MR, but methylpyrazine was not detected in control. Amounts of 2-methylbutanal, 3-methylbutanal, dimethyl disulfide, methylpyrazine, dimethyl trisulfide, methional, and 2-furanmethanol having positive odors (dark chocolate-, garlic-, hazelnut-, cooked potato-like) were 11.04, 50.15, 3.25, 8.38, 4.60, 9.59, and 3.08 times higher, respectively, in MR than those in raw.

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.

Measurements of Trimethylamine (TMA) in air by Tedlar bag sampling and SPME analysis (환경대기 중 Trimethylamine (TMA)의 측정: Tedlar bag 방식의 채취와 SPME 분석법의 특성 연구)

  • Kim, K.H.;Hyum, S.H.;Im, M.S.
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.96-102
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    • 2006
  • Trimethylamine (TMA) is one of the difficult odorous compounds for the collection and analysis. Although sulfuric acid absorption and/or sulfuric acid impregnated filter method are commonly recommended for its sampling, these methods also suffer from difficulties involved in sample treatment and operational procedures. Hence, as an ancillary approach to measure TMA, we investigated the combination of bag sampling and SPME analysis for TMA measurements. For the purpose of our study, we investigated the following three subjects: 1) temporal variability of standard storage, 2) bag loss effect of TMS, and 3) TMA loss due to repetitive analysis of an identical bag sample. According to our storage test up to 7 or 20 dyas, TMA loss were found to occur up to 40 to 50% within relatively short period of up to 48 hrs depending on its concentration ranges. When the tests were made for bag loss by transferring TMA standards across different size bags, we were able to find that the extent of bag loss are not significant with 5 to 20% loss rate. Finally, the TMA sorptive loss via its exposure to SPME fiber was generally estimated to run from 2 to 3%.

Analysis of Haloacetic Acids in Drinking Water by Direct Derivatization and Headspace-SPME Technique with GC-MS (Handspace Solid Phase Microextraction 방법에 의한 HAAs 분석에 관한 연구)

  • Cho, Deok-Hee
    • Journal of Korean Society of Water and Wastewater
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    • v.18 no.5
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    • pp.638-648
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    • 2004
  • In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

Determination of Aroma Components in Pinus densiflora (Pine Needles) Studied by Using Different Extraction Methods (추출방법에 따른 솔잎의 휘발성 성분 조성 비교)

  • Lee Jae-Gon;Lee Chang-Gook;Baek Shin;Kwon Young-Ju;Jang Hee-Jin;Kwag Jae-Jin;Rhee Moon-Soo;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.19 no.2
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    • pp.161-168
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    • 2006
  • The efficiency of six different extraction methods for the analysis of aroma components from pine needle(P. densiflora) was compared by gas chromatography-mass selective detector(GC-MSD). The six methods were dynamic headspace(DHS), reduced pressure headspace(RPHS), solid-phase microextraction(SPME), simultaneous distillation-extraction(SDE), supercritical fluid extraction(SFE) and pyrolysis distillation extraction(PDE). A total of 65 compounds were identified by using the six different extraction methods. These compounds are classified into six categories in terms of chemical functionality: 25 hydrocarbons, 16 alcohols, 9 carbonyls, 6 esters, 7 acids, and 2 ethers. The aroma compounds having low boiling point were more abundant in DHS, RPHS, and SPME extracts. On the other hand, the aroma compounds having high boiling point were more abundants in SDE, SFE and PDE extracts. The acid compounds were extracted by heat-based extraction methods such as SDE, SFE, PDE, but not by DHS, RPHS and SPME, which used neither solvent nor heat. The oxygenated terpens, hexanal, hexanol, and hexadienal were more abundant in DHS and RPHS extracts, compared with the other methods.