• Title/Summary/Keyword: HS-GC-MS

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A study on the development of phthalate plasticizers CRM in ABS resin (ABS 중 phthalates 가소제 CRM 개발에 대한 연구)

  • Jung, Jung-Sul;Park, Jung-Woo;Yoo, Seok;Kweon, Seong-Il;Hong, Sung-Taeg;Sun, Yle-Shik;Park, Cheon-Min;Choi, Chang-Hyoo
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.273-283
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    • 2012
  • Phthalate plasticizers are regulated by RoHS, REACH and CPSC as hazardous substances. Responding to these international environmental restrictions, we developed ABS certified reference material (CRM) for determination of phthalate plasticizers such as DMP, DEP, DBP, BBP, DEHP and DnOP. The candidate material has been made with ABS resin widely used in electric and electronic products and 6 kinds of phthalate plasticizers. The making of the material involved a series of processes like extruding, cooling, pelletizing, and drying using twin screw extruder. Then it has been certified according to ISO Guide 35. Using isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS), homogeneity, short-term stability, and long-term stability were evaluated. The certified values were determined by using primary reference material (PRM) of KRISS for traceability. From now on, we will provide ABS CRM to national and international companies and research institutes after certification as certified reference material and registering on COMAR (code of reference material).

Analysis of Volatile Organic Compounds in Sediments Using HS-GC/MS - Confirmation of Matrix Effects in External and Internal Standard Methods - (HS-GC/MS를 이용한 퇴적물 중 휘발성유기화합물 분석 - 외부 및 내부표준방법에서 매질영향 확인 -)

  • Shin, Myoung-Chul;Jung, Da-som;Noh, Hye-ran;Yu, Soon-ju;Seo, Yong-Chan;Lee, Bo-Mi
    • Journal of Korean Society on Water Environment
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    • v.37 no.6
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    • pp.510-519
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    • 2021
  • Volatile Organic Compounds (VOCs) in sediments, which can cause human health problems, have been monitored in Korea since 2014. Measured VOC concentrations can be affected by matrix type and the volatility of target substances. In this study, (1) VOCs volatility and the influence of matrix interference were confirmed, and (2) internal standards (IS) method was applied to improve analytical method. For these purposes, method detection limit (MDL), calibration linearity, precision and accuracy of VOCs were compared in various matrices using the IS. Some of VOCs in sediments showed different peak areas and reduced rates compared to water matrix. It was suggested that adsorption properties of sediments hindered the migration to vapor during heat pretreatment in headspace method. A calibration curve was created in clean sand. Recovery rates for the calibration curve method and IS applying method were 64.1~83.1% and 99.1~119.3%, respectively. Relative standard deviations ranged from 11.1% to 21.6% for the calibration curve method and those for IS ranged 4.7% to 13.7%. In case of real sediment, calibration curve and 1,2-Dichlorobenzene-d4 (ODCB) among IS were not suitable. The average recovery rate of Fluorobenzene (FBZ) increased by 56.4% and Relative Standard Deviation (RSD) by 4.7%. However, the recovery rate was increased in the samples with large values of igniting intensity. This study confirmed that influence of the matrix of VOCs in sediment, and addition of IS materials improved precision and accuracy. Although IS corrects volatilization and adsorption, it is recommended that more than two types of IS should be added rather than single.

Volatile Analysis of Commercial Korean Black Raspberry Wines (Bokbunjaju) Using Headspace Solid-phase Microextraction (Headspace Solid-phase Microextraction을 이용한 시판 복분자주의 휘발성분 분석)

  • Lee, Seung-Joo
    • Korean Journal of Food Science and Technology
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    • v.46 no.4
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    • pp.425-431
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    • 2014
  • In this study, the volatile compounds in 24 commercial Korean black raspberry wines were isolated by headspace solid-phase microextraction and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 43 volatile components, including 15 esters, 12 terpenes, 7 alcohols, 4 acids, 3 ketones, and 2 aldehydes, were identified. Ethyl esters and alcohols such as ethyl acetate, ethyl octanoate, isoamyl alcohol, and phenethyl alcohol were the most represented groups among the quantified volatiles. In particular, various terpenes such as DL-limonene, linalool, alpha-terpineol, and myrtenol were identified. The differences in volatile components among the 24 black raspberry wines and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 43.9% of the total variation across the samples. No apparent sample groupings were observed according to manufacturing locations. The samples KU, BH, SR, and MO showed higher overall levels in the concentrations of terpenes originating from black raspberry, while other samples such as BB and HB, showed higher in ethyl ester and alcohol contents produced by yeast fermentation, respectively.

Roasting and Cryogenic Grinding Enhance the Antioxidant Property of Sword Beans (Canavalia gladiata)

  • Jung, Ju-Yeong;Rhee, Jin-Kyu
    • Journal of Microbiology and Biotechnology
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    • v.30 no.11
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    • pp.1706-1719
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    • 2020
  • The objective of this study was to optimize the conditions for enhancing the antioxidant properties of sword bean (Canavalia gladiata) as a coffee substitute in two processing methods, roasting and grinding. The optimum conditions for removing off-flavor of the bean and maximizing functionality and efficiency were light roasting and cryogenic grinding (< 53 ㎛). In these conditions, extraction yield was 16.75%, total phenolic content (TPC) was 69.82 ± 0.35 mg gallic acid equivalents/g, and total flavonoid content (TFC) was 168.81 ± 1.64 mg quercetin equivalents/100 g. The antioxidant properties were 77.58 ± 0.27% for DPPH radical scavenging activity and 58.02 ± 0.76 mg Trolox equivalents/g for ABTS radical scavenging activity. The values for TFC and ABTS radical scavenging activity were significantly higher (p < 0.05) than in other conditions, and TPC and DPPH radical scavenging activity were second highest in lightly roasted beans, following raw beans. HS-SPME/GC-MS analysis confirmed that the amino acids and carbohydrates, which are the main components of sword bean, were condensed into other volatile flavor compounds, such as derivatives of furan, pyrazine, and pyrrole during roasting. Roasted and cryogenically ground (cryo-ground) sword beans showed higher functionality in terms of TFC, DPPH, and ABTS radical scavenging activities compared to those of coffee. Overall results showed that light roasting and cryogenic grinding are the most suitable processing conditions for enhancing the bioactivity of sword beans.

Effects of Glucose and Acrylic acid Addition on the Biosynthesis of Medium-Chain-Length Polyhydroxyalkanoates by Pseudomonas chlororaphis HS21 from Plant Oils (Pseudomonas chlororaphis HS21에 의한 식물유로부터 Medium-Chain-Length Polyhydroxyalkanoates 생합성이 미치는 포도당 및 아크릴산의 첨가 효과)

  • Chung Moon-Gyu;Yun Hye Sun;Kim Hyung Woo;Nam Jin Sik;Chung Chung Wook;Rhee Young Ha
    • Korean Journal of Microbiology
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    • v.41 no.3
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    • pp.225-231
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    • 2005
  • The characteristics of cell growth and medium-chain-length polyhydroxyalkanoate (MCL-PHA) biosynthesis of Pseudomonas chlororaphis HS21 were investigated using plant oils as the carbon substrate. The organism was efficiently capable of utilizing plant oils, such as palm oil, corn oil, and sunflower oil, as the sole carbon source for growth and MCL-PHA production. When palm oil (5 g/L) was used as the carbon source, the cell growth and MCL-PHA accumulation of this organism occurred simultaneously, and a high dry cell weight (2.4 g/L) and MCL-PHA ($40.2\;mol{\%}$ of dry cell weight) was achieved after 30 hr of batch-fermentation. The repeating unit in the MCL-PHA produced from palm oil composed of 3-hydroxyhexanoate ($7.0\;mol{\%}$), 3-hydroxyoctanoate ($45.3\;mol{\%}$), 3-hydroxydecanoate ($39.0\;mol{\%}$), 3-hydroxydodecanoate ($6.8\;mol{\%}$), and 3-hydroxytetradecanoate ($1.9\;mol{\%}$), as determined by GC/MS. Even though glucose was a carbon substrate that support cell growth but not PHA production, the conversion rate of palm oil to PHA was significantly increased when glucose was fed as a cosubstrate, suggesting that bioconversion of some functionalized carbon substrates to related polymers in P chlororaphis HS21 could be enhanced by the co-feed of good carbon substrates for cell growth. In addition, the change of compositions of repeating units in MCL-PHAs synthesized from the plant oils was markedly affected by the supplementation of acrylic acid, an inhibitor of fatty acid ${\beta}-oxidation$. The addition of acrylic acid resulted in the increase of longer chain-length repeating units, such as 3-hydroxydodecanoate and 3-hydroxytetradecanoate, in the MCL-PHAs produced. Particularly, MCI-PHAs containing high amounts of unsaturated repeating units could be produced when sunflower oil and corn oil were used as the carbon substrate. These results suggested that the alteration of PHA synthesis pathway by acrylic acid addition can offer the opportunity to design new functional MCL-PHAs and other unusual polyesters that have unique physico-chemical properties.

Composition and Cell Cytotoxicity of Essential Oil from Caryopteris incana Miq. in Korea (층꽃나무(Caryopteris incana Miq) 정유의 성분 분석과 세포 독성 평가)

  • Kim, Song-Mun
    • Applied Biological Chemistry
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    • v.51 no.3
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    • pp.238-244
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    • 2008
  • The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

Development of an analytical method of organochlorine pesticides in human bloods using head space-solid phase microextraction coupled with gas chromatography/mass spectrometry (HS SPME-GC/MS를 이용한 혈액 중 유기염소계 농약의 분석법 개발)

  • Kang, Tae-Woo;Pyo, Hee-Soo;Hong, Jong-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.259-271
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    • 2008
  • The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with $85{\mu}m$, adsorption time was for 5 min, adsorption optimum temperature was at $280^{\circ}C$, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs.

Evaluating the Headspace Volatolome, Primary Metabolites, and Aroma Characteristics of Koji Fermented with Bacillus amyloliquefaciens and Aspergillus oryzae

  • Seo, Han Sol;Lee, Sunmin;Singh, Digar;Park, Min Kyung;Kim, Young-Suk;Shin, Hye Won;Cho, Sun A;Lee, Choong Hwan
    • Journal of Microbiology and Biotechnology
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    • v.28 no.8
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    • pp.1260-1269
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    • 2018
  • Production of good Koji primarily depends upon the selection of substrate materials and fermentative microflora, which together influence the characteristic flavor and aroma. Herein, we performed comparative metabolomic analyses of volatile organic compounds (VOCs) and primary metabolites for Koji samples fermented individually with Bacillus amyloliquefaciens and Aspergillus oryzae. The VOCs and primary metabolites were analyzed using headspace solid phase microextraction (HS-SPME) followed by gas chromatography time-of-flight mass spectrometry (GC-TOF-MS). In particular, alcohols, ketones, and furans were mainly detected in Bacillus-fermented Koji (Bacillus Koji, BK), potentially due to the increased levels of lipid oxidation. A cheesy and rancid flavor was characteristic of Bacillus Koji, which is attributable to high content of typical 'off-flavor' compounds. Furthermore, the umami taste engendered by 2-methoxyphenol, (E,E)-2,4-decadienal, and glutamic acid was primarily detected in Bacillus Koji. Alternatively, malty flavor compounds (2-methylpropanal, 2-methylbutanal, 3-methylbutanal) and sweet flavor compounds (monosaccharides and maltol) were relatively abundant in Aspergillus-fermented Koji (Aspergillus Koji, AK). Hence, we argue that the VOC profile of Koji is largely determined by the rational choice of inocula, which modifies the primary metabolomes in Koji substrates, potentially shaping its volatolome as well as the aroma characteristics.

Functional Characterization of khadi Yeasts Isolates for Selection of Starter Cultures

  • Motlhanka, Koketso;Lebani, Kebaneilwe;Garcia-Aloy, Mar;Zhou, Nerve
    • Journal of Microbiology and Biotechnology
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    • v.32 no.3
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    • pp.307-316
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    • 2022
  • Yeasts play an important role in spontaneous fermentation of traditional alcoholic beverages. Our previous study revealed that a mixed-consortia of both Saccharomyces and non-Saccharomyces yeasts were responsible for fermentation of khadi, a popular, non-standardized traditional beverage with an immense potential for commercialization in Botswana. Functional characterization of isolated fermenting yeasts from mixed consortia is an indispensable step towards the selection of potential starter cultures for commercialization of khadi. In this study, we report the characterization of 13 khadi isolates for the presence of brewing-relevant phenotypes such as their fermentative capacity, ability to utilize a range of carbon sources and their ability to withstand brewing-associated stresses, as a principal step towards selection of starter cultures. Khadi isolates such as Saccharomyces cerevisiae, Saccharomycodes ludwigii and Candida ethanolica showed good brewing credentials but Lachancea fermentati emerged as the isolate with the best brewing attributes with a potential as a starter culture. However, we were then prompted to investigate the potential of L. fermentati to influence the fruity aromatic flavor, characteristic of khadi. The aroma components of 18 khadi samples were extracted using headspace solid phase micro-extraction (HS-SPME) and identified using a GC-MS. We detected esters as the majority of volatile compounds in khadi, typical of the aromatic signature of both khadi and L. fermentati associated fermentations. This work shows that L. fermentati has potential for commercial production of khadi.

Comparative Profiling of Volatiles in Flower Tea of Dendranthema zawadskii var. latilobum, Chrysanthemum morifolium, Tagetes erecta, and Matricaria chamomilla (구절초, 국화, 마리골드 및 캐모마일 꽃차의 향기 성분 비교)

  • Kanphassorn Wimonmuang;Young-Sang Lee;Seung-Young Oh;Suk-Keun Park
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2020.08a
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    • pp.109-109
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    • 2020
  • 꽃차(Flower tea)는 최근 다양한 제품이 개발되고 소비가 확대되는 등 그 산업적 가치가 증대하고 있다. 꽃차의 향기 특성은 우렸을 때 나타나는 색깔 및 인체에서의 생리활성과 더불어 주요한 꽃차 품질결정 요소이다. 본 연구는 꽃차로의 이용이 활발한 국화과 식물 중 구절초(Dendranthema zawadskii var. latilobum), 국화(Chrysanthemum morifolium), 노랑색 및 주황색 마리골드(Tagetes erecta 'Yellow' and 'Orange'), 그리고 캐모마일(Matricaria chamomilla)의 향기 성분특성을 구명하기 위하여 제조된 꽃차를 headspace-solidphase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS)를 이용하여 분리, 동정하였다. 국화과 꽃차로부터 총 117종의 휘발성 성분이 확인되었는데, 각 꽃차 종류별 동정된 휘발성 성분의 개수, 주요 3개 휘발성 성분과 전체 향기성분 peak중 이들이 차지하는 구성비율(%)은 다음과 같았다: 구절초 64종, camphor (31%), α-pinene(14%), camphene(14%); 국화 60종, camphor(15%), chrysantheny acetate(13%), eucalyptol (11%); 마리골드 '옐로우' 53종, 2,4-heptadienal(26%), trans-isocarveol(21%), cis-β-Copaene(18%); 마리골드 '오렌지' 61종, β-caryophyllene(16%), β-ocimene epoxide(12%), β-ocimene(12%); 캐모마일 50종, β-farnesene(63%), nonane(9%), spathulenol(5%). 국화과 꽃차 5종 모두에서 공통적으로 검출된 성분은 β-caryophyllene, α-pinene, β-farnesene 등 10종이었으며 마리골리 '옐로'는 '오렌지'와 주요 향기성분의 조성에서 뚜렷한 차이를 나타내었다. 비록 그 함량은 낮았으나 구절초, 국화, 마리골드 '오렌지', 그리고 캐모마일은 각각 10종, 12종, 3종 및 13종이었다. 마리골드 '엘로'의 경우 검출된 모든 향기성분은 마리골드 '오렌지'나 다른 국화과 식물의 꽃차에서도 검출된 바, 향기 성분이 다양성이 다소 낮게 나타났다.

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