• Title/Summary/Keyword: headspace sampling

Search Result 23, Processing Time 0.02 seconds

A Comparison of Different Extraction Methods for the Volatile Components of Anise(Pimpinella anisum L.) (추출방법에 의한 아니스의 휘발성 성분 조성 비교)

  • Kown, Young-Ju;Jang, Hee-Jin;Kwag, Jae-Jin;Kim, Ok-Chan;Choi, Young-Hyun;Lee, Jae-Gon
    • Applied Biological Chemistry
    • /
    • v.40 no.2
    • /
    • pp.144-147
    • /
    • 1997
  • Different isolation methods for the volatile components of Anise(Pimpinella anisum L.) are compared in terms of the difference of components obtained with each analytical procedure. These methods include headspace(purge & trap) sampling procedure, simultaneous distillation extraction(SDE), steam distillation and solvent extraction. Total 43 components were identified by? comparing gas chromatography retention time and mass spectral data. Different isolation techniques result in compositionally different isolates. The headspace(purge & trap) sampling procedure was found to be the best method of choice for a qualitative analysis of the volatile components.

  • PDF

Analysis of Volatiles in Sesame Oil Collected by Simultaneous Distillation/Extraction(SDE) and Dynamic Headspace Sampling (DHS) (연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)에 의한 참기름 중의 향기성분의 분석)

  • Ha, Jaeho
    • Analytical Science and Technology
    • /
    • v.9 no.4
    • /
    • pp.399-405
    • /
    • 1996
  • The flavor compounds of the oil from roasted sesame seeds were collected by simultaneous steam distillation/ extraction(SDE) and dynamic headspace sampling(DHS) and were analyzed using a gas chromatograph equipped with a flame ionization detector and connected into a mass spectrometer. Among the flavor compounds collected by the SDE method, 46 compounds were identified. They consisted of 6 alcohols, 6 aldehydes, 5 ketones or acids, 4 furans or phenols, 12 pyrazines, 4 pyridines or thiazoles, and others. Thirty six compounds were identified by DHS and many of them were the same as those identified by the SDE method. However, some compounds such as 1-hexanol, pentanal, and dimethylsulfide were identified only by the DHS method.

  • PDF

Optimization of Headspace Sampling Using Solid Phase Microextraction For Volatile Organic Acids in Different Tobacco Types

  • Lee, Jang-Mi;Lee, Jeong-Min;Son, Seong-Ae;Kwon, Young-Ju;Jang, Gi-Chui;Kim, Young-Ho
    • Journal of the Korean Society of Tobacco Science
    • /
    • v.35 no.1
    • /
    • pp.7-12
    • /
    • 2013
  • A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.

Rapid Determination of Volatile Organic Compounds in Human Whole Blood Using Static Headspace Sampling with Gas Chromatography and Mass Spectrometry

  • Lee, Ji-Young;Kim, Seungki;Lee, Jong-Tae;Choi, Jong-Ho;Lee, Jeongae;Pyo, Heesoo
    • Bulletin of the Korean Chemical Society
    • /
    • v.33 no.12
    • /
    • pp.3963-3970
    • /
    • 2012
  • Headspace (HS) and headspace solid-phase microextraction (HS-SPME) were studied for extracting volatile organic compounds (VOCs) from whole blood, with chemical and instrumental variables being optimized for maximum sensitivity: incubation at $60^{\circ}C$, equilibration for 30 min, pH 11, and 2 mL injection volume. Both techniques provided accurate analyses, with detection limits of 0.05-0.1 ng $mL^{-1}$ and 0.05-0.5 ng $mL^{-1}$. HS showed better sensitivity, reproducibility, and analysis times than HS-SPME. Overall levels of chloroform in whole blood were found to be 0.05-5.84 ng $mL^{-1}$; detected levels of benzene were 0.05-2.20 ng $mL^{-1}$.

Studies on Volatile Compounds in Lipoxygenase Deficient-soybean and Its Products (Lipoxygenase 결핍 콩과 그 가공품의 휘발성 성분 분석)

  • 김수희;이양봉;황인경
    • The Korean Journal of Food And Nutrition
    • /
    • v.13 no.2
    • /
    • pp.118-124
    • /
    • 2000
  • Lipoxygenase(LOX) in soybeans is responsible for beany flavors which limit the wide utilization of soybeans to foods. This study was conducted to analyze beany flavor compounds of the normal Hwagkeumkong and LOX-deficient soybean cultivars, Jinpumkong which lacks L-2, L-3, and Jinpumkong 2 which lacks all L-1, L-2, L-3. Using the combination of dynamic headspace sampling and gas chromatography-mass selective detector(DHS-GC-MSD) for analyzing volatile compounds, hexanal and hexanol were identified in whole soy flour of all three soybena cultivars. Hwangkeumkong had more volatile compounds than Jinpumkong and Jinpumkong 2 in defatted soy flour. Hexanal and acetic acid were identified in soy milk of all three soybean cultivars but Hwangkeumkong had more volatile compounds than Jinpumkong 2. From the analysis with a static headspace sampling(SHS) and GC-MSD the major compounds were hexanal, acetic acid, 1-hexanol, and 1-octen-3-ol. The content of acetic acid was similar among three cultivars. But contents of hexanal and pentanal in Jinpumkong 2 were less than that of Jinpumkong and Hwangkeumkong. Using GC-FID, Jinpumkong 2 had less contents of hexanal and pentanol than Hwangkeumkong in whole soy flour and defatted soy flour. In this study, LOX-deficient soybean cultivars showed less hexanal, pentanol and other compounds than the normal Hwangkeumkong. However quite amount of beany flavor compounds were identified in Jinpumkong and Jinpumkong 2. So further studies are required to characterize LOX isozymes, to understand the mechanisms of beany flavors production, and to develop some other methods for removing beany flavor.

  • PDF

Analysis of Flavor Composition of Coriander Seeds by Headspace Mulberry Paper Bag Micro-Solid Phase Extraction

  • Cha, Eun-Ju;Won, Mi-Mi;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
    • /
    • v.30 no.11
    • /
    • pp.2675-2679
    • /
    • 2009
  • This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

Studies on Measuring Volatile Terpenoids in Carrots Using the Direct Headspace Sampling Method (Direct Headspace Sampling 방법을 이용한 당근의 휘발성 Terpenoids 분석에 관한 연구)

  • Park, Yong;Ryu, Jang-Bal;Park, Sang-Gyu;Park, Shin
    • Applied Biological Chemistry
    • /
    • v.40 no.6
    • /
    • pp.536-540
    • /
    • 1997
  • Volatile terpenoids of carrots were measured by the direct headspace sampling method(DHS) with gas chromatography as a study for the breeding of high quality carrots. Using this method, 7 terpenoids such as ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, ${\alpha}-terpinene$, limonene, ${\gamma}-terpinene$, and terpinolene were clearly separated. However ${\alpha}-phellandrene$ was not clearly separated from ${\beta}-myrcene$. In addition to this, higher boiling point compounds such as terpinen-4-ol, bornyl acetate, and ${\alpha}-bisbolol$ were not found. The coefficients of $determination(r^2)$ for the 7 terpenoids were higher than 0.99 and the standard curves were highly significant. Four replicated samples using this method demonstrated great reproducibility; the coefficidnt of variation (C.V.) for ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, limonene, ${\gamma}-terpinene$, terpinolene, and total terpenoids were 6.8, 6.8, 8.4, 7.1, 3.8, 10.1, 7.1%. Sixty five carrot cultivars breeded worldwide were evaluated for the 7 terpenoids and total terpenoids; the range for ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, ${\alpha}-terpinene$, limonene, ${\gamma}-terpinene$, terpinolene, and total terpenoids were $0.28{\sim}2.48\;ppm$, $0.35{\sim}1.87\;ppm$, $0.56{\sim}1.51\;ppm$, 0 ppm, $0.59{\sim}1.84\;ppm$, $0.87{\sim}3.33\;ppm$, $5.15{\sim}35.81\;ppm$, and $9.07{\sim}42.30\;ppm$, respectively. Big differences in each terpenoid and total terpenoids were found among cultivars. On the total terpenoids of the 65 cultivars, 5 cultivars(7.7%) contained less than 10 ppm, 15 cultivars (23.1%) $10{\sim}11.99\;ppm$, 14 cultivars(21.5%) $12{\sim}13.99\;ppm$, 9 cultivars(13.8%) $14{\sim}15.99\;ppm$, 10 cultivars(15.4%) $16{\sim}17.99\;ppm$, 4 cultivars(6.2%) $18{\sim}19.99\;ppm$, 5 cultivars(7.7%) $20{\sim}29.99\;ppm$, and 3 cultivars(4.6%) were higher than 30 ppm. Generally, cultivars developed in Japan contained less total terpenoids than cultivars developed in Europe and America.

  • PDF

Comparative Sampling Procedures for the Volatile Flavor Components of Codonopsis lanceolata (전처리 방법에 따른 더덕(Codonopsis lanceolata)의 휘발성 향기성분 비교 분석)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Kim, Jae-Jung;Oh, Chang-Hwan
    • Korean Journal of Food Science and Technology
    • /
    • v.24 no.2
    • /
    • pp.171-176
    • /
    • 1992
  • Volatile flavor components of Codonopsis lanceolata were extracted by gas co-distillation (GCD), solvent extraction/fractionation (SEF), and headspace sampling (HSS) methods. The extracts were analyzed by dual-capillary gas chromatography-retention index (GC-RI) and gas chromatography-mass spectrometry(GC-MS). The two extracts prepared by SEF and HSS gave more similar fragrance to the Codonopsis lanceolata than the GCD extract. The GC profiles of the SEF and HSS extracts were similar to each other except for differences in peak areas. The extract prepared by SEF gave a sweet note while the extract prepared by HSS gave a green note. The GCD extract began to give a burnt note of herb medicine with prolonged distillation. Rapid extraction of flavor components from Codonopsis lanceolata was possible in several short steps by SEF and HSS methods compared to GCD. GC-MS and GC-RI were used for peak identification. GC-RI was more effective for identification of isomers, and polar FFAP column was more suitable for identification of polar compounds. From Codonopsis lanceolata we identified 35 volatile flavor constituents, 24 of which have not been previously reported by simultaneous distillation extraction method $^{(5)}$. trans-2-Hexanal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, and hexanol were considered key components of the green note and 1-octen-3-ol, the component of the fresh note. Esters, including amyl propionate, seem to be responsible for the sweet note particular to Codonopsis lanceolata.

  • PDF

Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.1
    • /
    • pp.139-142
    • /
    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

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
    • /
    • v.54 no.3
    • /
    • pp.188-200
    • /
    • 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.