• Title/Summary/Keyword: headspace GC/MS

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Determination of geosmin and 2-MIB in Nakdong River using headspace solid phase microextraction and GC-MS (HS-SPME-GC/MS를 이용한 낙동강 수계 하천수 중 조류기원성 냄새물질 분석)

  • Lee, Injung;Lee, Kyoung-Lak;Lim, Tae-Hyo;Park, Jeong-Ja;Cheon, Seuk
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.326-332
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    • 2013
  • Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

Development of an Analytical Method for Chloropicrin Determination in Hulled Rice by GC-ECD and GC-MS (GC-ECD 및 GC-MS를 이용한 현미 중 chloropicrin의 잔류시험법 개발)

  • Do, Jung-Ah;Choi, Jeong-Heui;Park, Hyejin;Park, Yong-Chun;Yoon, Hae-Jung;Choi, Dongmi;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.28 no.3
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    • pp.222-226
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    • 2013
  • A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.

Analysis of Volatile Flavor Compounds in Milk Using Electronic Nose System (전자코 시스템을 이용한 우유의 품질에 따른 휘발성 향기성분 분석)

  • Kang, Nae Kyung;Jun, Tae-Sun;Yang, Yoon Seok;Kim, Yong Shin
    • Journal of Sensor Science and Technology
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    • v.23 no.5
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    • pp.320-325
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    • 2014
  • Volatile flavor compounds from milk were analyzed and identified by using the analysis methods of headspace solid phase microextraction gas chromatography/mass spectrometry (HSPME-GC/MS) and electronic nose (E-Nose) system. About 30 volatile compounds were identified by HSPME-GC/MS for the fresh and off-flavor milk samples. Also, the correlation between rancidity and ageing days of milk was obtained by the aid of principal component analysis algorithm. It shows that the E-Nose system can identify the various types of milk flavor. These results imply that the analysis method based on the E-nose system can apply to the quality control of milk flavor and the rancidity.

Volatile Component Analysis of Commercial Japanese Distilled Liquors (Shochu) by Headspace Solid-Phase Microextraction (헤드스페이스 고체상미량추출(Solid-Phase Microextraction)을 이용한 시판 일본소주의 휘발성 향기성분 분석)

  • Shin, Kwang-Jin;Lee, Seung-Joo
    • Korean Journal of Food Science and Technology
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    • v.47 no.5
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    • pp.567-573
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    • 2015
  • In this study, volatile compounds in nine commercial Japanese distilled liquors (Shochu) were isolated by headspace solid-phase microexrraction (SPME) and analyzed by gas chromatography (GC) and GC-mass spectrometry (MS). A total of 76 volatile components, including 48 esters, 13 alcohols, and 15 miscellaneous components, were identified. Esters and alcohols constituted the largest groups of quantified volatiles. Differences in volatile components among the distilled liquors and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 77.92% of the total variation across the samples. The samples using barley koji showed higher overall concentrations of total volatile components. Additionally, the principal component analysis did not reveal any sample grouping based on the raw material used.

A Study on Residual Amounts of Vinyl Chloride/Vinylidene Chloride in Poly(vinyl chloride)/Poly(vinylidene chloride) Food Packaging using Headspace GC/MS (헤드스페이스 GC/MS를 이용한 폴리염화비닐/폴리염화비닐리덴 식품 포장 중 염화비닐/염화비닐리덴 잔류량 연구)

  • Sung, Jun-Hyun;Kwak, In-Shin;Park, Sung-Kwan;Kim, Hyung-Il;Lim, Ho-Soo;Lee, Ju-Young;Byun, Mi-Yun;Kim, So-Hee
    • Korean Journal of Food Science and Technology
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    • v.43 no.1
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    • pp.6-11
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    • 2011
  • Vinyl chloride (VC) and vinylidene chloride (VDC), which may be present in poly(vinyl chloride) (PVC) and poly(vinylidene chloride) (PVDC) food packaging, were analyzed by using a headspace-gas chromatograph (GC)/mass spectrometer (MS) equipped with a PLOT Q column. 1-Chloropropane (1-CP) was used as an internal standard. The determinations of VC and VDC were carried out by monitoring the characteristic ions for each compound: m/z=61, 62, 64 and m/z=61, 96, 98, respectively. The method validated in this study can be suitable for the compliance test of EU regulation. Among 103 food packaging samples, VC and VDC were not detected, except in one PVDC food package. However, the detected level of VDC in the sample was below the EU regulatory specific limitation.

The Study on the Measurement of Formaldehyde in Hair by HS-GC-MS (헤드스페이스-가스크로마토그래피-질량분석법에 의한 체모 중 포름알데하이드 측정법 연구)

  • Shin Ho-Sang;Ahn Hye-Sil
    • Journal of Environmental Health Sciences
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    • v.32 no.1 s.88
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    • pp.67-70
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    • 2006
  • A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

Characterization of Fennel Flavors by Solid Phase Trapping-Solvent Extraction and Gas Chromatography-Mass Spectrometry

  • Shin, Yeon-Jae;Jung, Mi-Jin;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2389-2395
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    • 2007
  • Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

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 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.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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