• Title/Summary/Keyword: Solid Phase Microextraction-GC/MS

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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.

Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization (Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석)

  • Ahn, Yun Gyong;Lee, Jee Yeon;Kim, Jeehyeong;Hong, Jongki
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.458-465
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    • 2003
  • The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

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.

Evaluation of TVOC contribution from Raw materials of PVC wallpaper using the Headspace-SPME-GC/MS (HS-SPME-GC/MS 법을 이용한 PVC벽지 원자재의 TVOC 기여도 평가)

  • Jang, Mi-Ok;Jeong, Tak-Kyo;Jeong, Yung-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.488-495
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    • 2007
  • A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.

기체크로마토그래피-질량분석검출기와 고체상미량추출법을 이용한 물 중의 MTBE 미량분석

  • Jeon Chi-Wan;Lee Jeong-Hwa;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.195-198
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    • 2005
  • A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.

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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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Volatile organic compounds of pyroligneous liquor of bamboo sprout produced in damyang-gun (담양군 죽초액의 휘발성성분 분석)

  • Lee, Eunsil;Jang, Hyejin;Lee, Songjin;Ha, Jaeho
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.299-306
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    • 2013
  • Pyroligneous liquor as a byproduct from charcoal production of bamboo sprout produced damyang-gun has the broad benefits such as improvement of soil quality, plant growth control and is mainly used for the treatment of atopic dermatitis, fungi and many other skin diseases. In this study, flavor compounds of pyroligneous liquor from bamboo sprout produced in Damyang-gun were analyzed and compared using three different methods including direct analysis (DA), headspace solid phase microextraction (HS-SPME) and stir bar sorptive extraction (SBSE). Simultaneously, the analytical conditions of GC-MS for the determination of volatile compounds were optimized. Based on volatile organic compounds detected by GC-MS, SBSE and SPME methods showed higher sensitivity than direct analysis. Major compounds of pyroligneous liquor were cresol, guaiacol, p-ethyl guaiacol and syringol. These phenolic compounds are reported as the useful chemicals with medicinal activity.

Analysis of fatty acid methyl ester in bio-liquid by hollow fiber-liquid phase microextraction

  • Choi, Minseon;Lee, Soyoung;Bae, Sunyoung
    • Analytical Science and Technology
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    • v.30 no.4
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    • pp.174-181
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    • 2017
  • Bio-liquid is a liquid by-product of the hydrothermal carbonization (HTC) reaction, converting wet biomass into solid hydrochar, bio-liquid, and bio-gas. Since bio-liquid contains various compounds, it requires efficient sampling method to extract the target compounds from bio-liquid. In this research, fatty acid methyl ester (FAME) in bio-liquid was extracted based on hollow fiber supported liquid phase microextraction (HF-LPME) and determined by Gas Chromatography-Flame Ionization Detector (GC-FID) and Gas Chromatography/Mass Spectrometry (GC/MS). The well-known major components of biodiesel, including methyl myristate, palmitate, methyl palmitoleate, methyl stearate, methyl oleate, and methyl linoleate had been selected as standard materials for FAME analysis using HF-LPME. Physicochemical properties of bio-liquid was measured that the acidity was 3.30 (${\pm}0.01$) and the moisture content was 100.84 (${\pm}3.02$)%. The optimization of HF-LPME method had been investigated by varying the experimental parameters such as extraction solvent, extraction time, stirring speed, and the length of HF at the fixed concentration of NaCl salt. As a result, optimal conditions of HF-LPME for FAMEs were; n-octanol for extraction solvent, 30 min for extraction time, 1200 rpm for stirring speed, 20 mm for the HF length, and 0.5 w/v% for the concentration of NaCl. Validation of HF-LPME was performed with limit of detection (LOD), limit of quantitation (LOQ), dynamic range, reproducibility, and recovery. The results obtained from this study indicated that HF-LPME was suitable for the preconcentration method and the quantitative analysis to characterize FAMEs in bio-liquid generated from food waste via HTC reaction.

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.

Analysis of Flavor-related Compounds from Tobacco using SPME-GC-MS (SPME-GC-MS를 이용한 담배와 관련된 향료의 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.109-114
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    • 2001
  • The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry(GC-MS). Flavor-related compounds were estragole pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin. More than on of the flavor-related compounds were detected in the range $0.001-1.3{\mu}g/g$ from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%.

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