• 제목/요약/키워드: Solid-phase microextraction

검색결과 203건 처리시간 0.023초

고체상미세추출법(SPME)을 이용한 피혁 재질로부터 발생된 휘발성 유기화합물 분석기술 연구 (The Analysis on VOCs That Occurs in Leather Cultural Heritage with SPME)

  • 정용재
    • 보존과학회지
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    • 제28권2호
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    • pp.113-118
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    • 2012
  • 문화재는 화학적 요인, 생물학적 요인 등 각종 열화 인자에 의해 재질이 열화되면서 각각 특유의 휘발성 유기화합물을 방출해내며 이러한 휘발성 유기화합물은 대기 중에 존재하고 다른 재질로 이루어진 유물의 열화 인자로 작용한다. 하지만 다수의 분석법 중에 비파괴적인 분석법은 흔치 않으며 기기 사용의 어려움으로 현장적용에 어려움을 겪고 있다. 본 연구는 피혁에서 발생하는 유해가스를 비파괴적이고 조작이 간편한 고체상미세추출법과 기체크로마토그래피를 통해 분석을 실시하였다. 또한 고체상미세추출법 중 이동형 홀더(field holder)의 효율성을 입증하였다. 국가기록원에 보관 중인 행정박물 중 피혁으로 이루어진 유물을 선정하여 고체상미세추출법의 현장적용을 실시, 비교 분석함으로써 피혁재질에서 자체적으로 발생하여 주변 공기에 방출시키는 (E)-2-nonenal, butyl hydroxy toluene 등의 화합물을 확인할 수 있었다.

전자코와 GC/MS를 이용한 포도 품종별 저장 조건에 따른 휘발성 향기 성분 연구 (Identification of Volatile Compounds of 4 Grape Species by Storage Conditions)

  • 이윤정;이기택
    • 한국식품영양과학회지
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    • 제36권7호
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    • pp.874-880
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    • 2007
  • 품종에 따른 포도를 이용하여 3일 동안 $4^{\circ}C$와 실온에 각각 저장함에 따라 변화하는 전체적인 향의 패턴을 전자코를 통하여 분석하였고 SPME-GC/MS 분석 결과를 통하여 휘발성분을 분리 동정하였다. 대표적인 포도의 주요 휘발 성분은 alcohols, esters, acids, terpenes 등으로 GC/MS 분석 결과 butanoic acid/ethyl ester와 1-hexanol, hexanoic acid/ethyl ester, phenylethyl alcohol 등이 주요 성분으로 동정되었다. 캠벨은 다른 품종에 비해 다양한 휘발 성분이 동정되었고 레드글로브와 머루 품종에서는 1-hexanol, 2-decene, 8-methyl-(z)/1-dodecanol 등을 제외한 나머지 휘발 성분은 거의 나타나지 않았다. 또한 전자코를 이용하여 휘발성 향기성분 패턴 분석결과 $4^{\circ}C$와 실온 저장한 시료의 제 1주성분 값의 기여율은 각각 99.30, 99.36%로 품종에 따라 구분이 가능하였다. $4^{\circ}C$ 저장 시 저장 기간에 따른 제 1주성분 값의 변화 범위는 실온에서 저장한 것에 비해 적었음을 확인할 수 있었다.

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

  • 박교범;이석근
    • 분석과학
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    • 제14권2호
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    • pp.109-114
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    • 2001
  • 담배에 포함된 향료 성분을 headspace solid phase microextraction(SPME)를 이용하여 gas chromatography-mass spectrometry(GC-MS)의 selected ion monitoring(SIM)방법으로 분석하였다. 본 연구에서 사용한 담배향과 관련된 성분은 estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methylisoeugenol 및 myristicin 등 11종이며 분석결과 모든 담배에서 한가지 또는 그 이상의 담배향 성분을 $0.001-1.3{\mu}g/g$ 검출할 수 있었으며 회수율은 89.1-102.9%로 나타났고 상대표준편차는 2.6-25.2%를 얻었다.

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Development of New Surfaces and Materials for Separation Science

  • Linford, Matthew R.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2015년도 제49회 하계 정기학술대회 초록집
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    • pp.59.1-59.1
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    • 2015
  • In the Linford group at Brigham Young University we have recently developed three new sets of materials for three different areas of separations science: thin layer chromatography (TLC), high performance liquid chromatography (HPLC), and solid phase microextraction (SPME). First, via microfabrication we have grown patterned carbon nanotube (CNT) forests on planar substrates that we have infiltrated with inorganic materials such as silicon nitride. The coatings on the CNTs are conformal and typically deposited in a process like low pressure chemical vapor deposition. The resulting materials have high surface areas, are porous, and function as effective separation devices, where separations on our new TLC plates are typically significantly faster than on conventional devices. Second, we used the layer-by-layer (electrostatically driven) deposition of poly (allylamine) and nanodiamond onto carbonized poly (divinylbenzene) microspheres to create superficially porous particles for HPLC. Many interesting classes of molecules have been separated with these particles, including various cannabinoids, pesticides, tricyclic antidepressants, etc. Third, we have developed new materials for SPME by sputtering silicon onto cylindrical fiber substrates in a way that creates shadowing of the incoming flux so that materials with high porosity are obtained. These materials are currently outperforming their commercial counterparts. Throughout this work, the new materials we have made have been characterized by X-ray photoelectron spectroscopy, time-of-flight secondary ion mass spectrometry, scanning electron microscopy, transmission electron microscopy, etc.

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대학생들의 혈액 내 휘발성 유기화합물 노출에 영향을 미치는 요인 (Determinant Factors for Blood VOCs Exposures in College Students)

  • 최정미;김민수;신원호;문찬석
    • 한국환경보건학회지
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    • 제41권1호
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    • pp.24-29
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    • 2015
  • Objectives: The objective of this study was to identify determine factors for blood VOCs levels in college students. Methods: Venous blood samples were collected from healthy 29 male and 25 female volunteers. The samples were analyzed with solid-phase microextraction gas chromatography and mass spectrometry. Results: Blood concentrations of benzene, toluene, ethylbenzene, m-,p-xylene, o-xylene were higher in smoking group than in non-smoking group. Geometric means of smoking group and non-smoking group were 0.45 and $0.36{\mu}g/L$ in benzene, 0.82 and $0.47{\mu}g/L$ in toluene, 0.44 and $0.41{\mu}g/L$ in ethylbenzene, 0.49 and $0.39{\mu}g/L$ in m-,p-xylene and 0.47 and $0.43{\mu}g/L$ in o-xylene, respectively. Gender, alcohol drinking, coffee, commuting time (30 minutes) by a car and adjacency between home and road were not associated with increasing blood VOCs concentrations of college students. Conclusion: Smoking habit was significantly associated with blood concentrations of benzene, toluene, ethylbenzene, o-,m-,p-xylene in college students.

헤드스페이스-SPME 방법을 이용한 트리메틸아민의 분석방법 연구 (The Analysis of Airborne Trimethylamine Using a Headspace (HS)-SPME Method)

  • 안지원;김기현
    • 한국대기환경학회지
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    • 제24권3호
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    • pp.357-366
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    • 2008
  • In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

고도산화공정(UV공정)을 이용한 NDMA의 효율적인 처리와 독성 평가 (Effective Treatment of N-Nitrosodimethylamine using Advanced Oxidation Process (UV Process) and Toxicity Evaluation)

  • 송원용;장순웅
    • 한국물환경학회지
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    • 제25권1호
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    • pp.90-95
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    • 2009
  • This study investigates the oxidative degradation of N-nitrosodimethylamine (NDMA), a probable human carcinogen, by advanced oxidation process (i.e., UV process). The experiments were performed with various pH, initial concentration, UV intensity, and addition of $H_2O_2$ or $TiO_2$ on UV process. The results showed that the direct UV photolysis was the most effective treatment method. The lower pH, intial concentration and higher intensity of UV stimulated higher NDMA removal. However, addition of oxidant ($H_2O_2$, $TiO_2$) slows down photochemical treatment of NDMA since the oxidant can filter out the UV light and block it to reach the NDMA molecules. Dimethylamine (DMA) and nitrite were found to be a major byproduct from NDMA oxidation. To evaluate the chronic toxicity effects of UV-treated NDMA on the growth of microalgae, "Skeletonema costatum", was studied as long term experiments. Results demonstrated that after the 13 days exposure the chronic toxicity was decreased about 15% with application of UV process on NDMA degradation.

Quantitation of Formate in Plants and Its Enhancement in Response to Environmental Stresses

  • Kim, Jae-Kwang;Cho, Myoung-Rae;Baek, Hyung-Jin;Ryu, Tae-Hun;Kim, Jung-Bong;Kim, Jun-Heong;Kim, Myong-Jo;Yu, Chang-Yeon;Fukusaki, Ei-Ichiro;Kobayashi, Akio
    • Journal of Applied Biological Chemistry
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    • 제50권4호
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    • pp.211-214
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    • 2007
  • A solid-phase microextraction and gas chromatography-mass spectrometry utilizing $^{13}C$-formate as an internal standard for the determination of formate was proved to be applicable as a reliable quantitative method in several plants. We were the first to discover that trees contain larger pool sizes of formate than herbs. Our data also showed that the formate level of the leaves increased after the methanol-spraying, suggesting that methanol oxidation could convert formaldehyde into formate. In addition, drought and chilling led to the increase of endogenous formate in Arabidospsis thaliana. These results confirmed that formate is a universal stress signal in plants.

Comparative Study on Volatile Flavor Compounds of Traditional Chinese-type Soy Sauces Prepared with Soybean and Defatted Soy Meal

  • Gao, Xian-Li;Zhao, Hai-Feng;Zhao, Mou-Ming;Cui, Chun;Ren, Jiao-Yan
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1447-1458
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    • 2009
  • Volatile extracts obtained from traditional Chinese-type soy sauces prepared with soybean (SSSB) and defatted soy meal (SSDSM) by solid phase microextraction (SPME) and direct solvent extraction (DSE) were analyzed by gas chromatography-mass spectrometry (GC-MS). The volatile flavor compounds and relative contents of different chemical classes detected in SSSB and SSDSM were compared for their differences. Results showed that significant differences in both constituents of volatile flavor compounds and relative contents of different chemical classes were observed for both kinds of soy sauces. A total of 152 and 131 compounds were identified in SSSB and SSDSM, respectively, and 102 volatile flavor compounds were common in both kinds of soy sauces. Moreover, relative contents of acids, aldehydes, esters, furan(one)s, miscellaneous compounds, phenols, pyrazines, pyrrol(idinon)es, and sulfur-containing compounds in both kinds of soy sauces were all significantly different.

Impact of High Temperature on the Maillard Reaction between Ribose and Cysteine in Supercritical Carbon Dioxide

  • Xu, Honggao;He, Wenhao;Liu, Xuan;Gao, Yanxiang
    • Food Science and Biotechnology
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    • 제18권1호
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    • pp.66-72
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    • 2009
  • An aqueous ribose-cysteine model system (initial pH 5.6) was conventionally heated to the same browning at varying temperatures ($120-180^{\circ}C$), supercritical carbon dioxide (SC-$CO_2$, 20 MPa) was also applied on the same matrices for same periods at each temperature and about 20% reduction of the absorbance at 420 nm was observed as compared with sole thermal treatment. The headspace volatiles from Maillard reaction mixtures were analyzed by solid-phase microextraction (SPME) in combination with gas chromatography and mass spectrometry (GC-MS), and predominated with sulfur containing compounds, such as thienothiophenes, polysulfur alicyclics, thiols, and disulfides. Reaction temperature exhibited complex effects on volatiles formation and those effects became further complicated by the SC-$CO_2$ treatment. The formation of noncarbonyl polysulfur heterocyclic compounds and thienothiophenes was generally favored at high temperatures. Most volatiles were inhibited in SC-$CO_2$ as compared with thermal treatment alone, however, the well-known meaty aromatic compounds, such as thiols and disulfides, were obviously enhanced.