• Title/Summary/Keyword: silylation

Search Result 38, Processing Time 0.024 seconds

Quantitative Analysis of Pentachlorophenol in Paper Products (종이재 중의 Pentachlorophenol 정량 분석)

  • Hahn, Airan;Park, Jihye;Choi, Hyeongki;Hong, Sungyeap;Han, Hyechul;Jo, Byoungmuk;Oh, Jungsoo
    • Applied Chemistry for Engineering
    • /
    • v.16 no.3
    • /
    • pp.323-327
    • /
    • 2005
  • Pentachlorophenol (PCP) is a representative compound of chlorophenol derivatives which are especially toxic and potentially carcinogenic compounds in the priority pollutant list of the EPA (Environmental Protection Agency, USA). The aim of this study was to investigate an analysis method of PCP in infinitesimal quantity retained in paper. PCP in paper was pretreated by solid phase extraction (SPE) in a phenyl cartridge. The extracted sample was acetylated or silylated and analyzed with GC/MS-SIM. The detection sensitivity of silylated PCP was improved significantly when compared with those of PCP itself and acetylated PCP. As a test specimen, an office paper and a wallpaper were used.

Studies of Duvatrienediol in Tobacco Leaf (Nicotiana tabacum L.) (잎담배중 Duvatrienediol에 관한 연구)

  • 지상운;안기영;이문수;박영수;정찬선
    • Journal of the Korean Society of Tobacco Science
    • /
    • v.14 no.2
    • /
    • pp.159-167
    • /
    • 1992
  • It would be clear that the constituents of the leaf surface lipid is ye비 important as an evaluation index of tobacco leaf quality since the quality of tobacco specific aroma with leaf species depends on the contents of the lipid and the strength of the aroma is determined by the amounts of the lipid secreted. For the reason, a rapid and peproducible method to quantify DVT, which is a kind of lipid, has been studied. The biosynthesis procedure of DVT in leaf growing processes, and the volatile or decompositional characters of DVT in leaf drying processes were also discussed. In consequence, it might be possible to get the data available to the cultivation of better tobacco leaf and the manufacture of cigarettes with better aroma and taste. The results obtained from this study are as follows. 1. Chloroform/dichloromethane solvent was better than chloroform alone for DVT extraction. The extraction yields of the leaf surface lipid were about 5% 2. The extractives with dichloromethane were treated by silylation with BSTPa and the quantitative analysis of DVT was carried out using SE -54 fused silica capillary column. It was found that rapid and reproducible data could be obtained from these methods. 3. In flue - cured tobacco species, DVT contents were $30.3\mu\textrm{g}/cm^2$ in the beginning stage of leaf drying processes and $12.1\mu\textrm{g}/cm^2$ corresponded to 30% levels of the beginning stage, in the end stage. 4. DVT contents in Burley mere 2 times as large as those in fluecured tobacco. DVT in the upper stalk position of leaf was 3 times larger than that in the lower stalk position. 5. DVT of tobacco leaves was decomposed by $SO_2$ gas or the sun light. The decomposition rate was largest in the sample used methanol as a extraction solvent.

  • PDF

The Microdetermination of Ascorbic acid in Blood by Gas-Liquid Chromatography (혈액중(血液中) Ascorbic acid 의 Gas-Liquid Chromatography 에 의(依)한 미량정량(微量定量))

  • Lee, Joong-Hee
    • Applied Biological Chemistry
    • /
    • v.18 no.1
    • /
    • pp.52-55
    • /
    • 1975
  • A microdetermination of Ascorbic acid (AsA) in blood by Gas-Liquid Chromatography (GLC) was studied. AsA was applied on GLC after the conversion into trimethylsilyl derivative (TMS) and the GLC was available for the only reduced form of AsA. A calibration curve is made by GLC of TMS-AsA as the internal standard of n-docosane. The minimum amount of AsA required for the determination was 0.5ml of 1 mg% pyridine solution. Prior to the conversion of AsA in serum into TMS derivative, serum was lyophilized and then it was allowed to stand at room temperature with TMS reagents for 48 hr. On injection of the supernates of TMS derivative to GLC the peak corresponding to AsA was not detected. Its reason why the concentration of AsA in serum is $0.5mg{\sim}0.8mg%$ in general, and it is less than minimum concentration of GLC. In case of L-AsA 1 mg was added to 1ml of serum, which was followed by lyophilization, silylation and GLC. The recorvery of AsA added was 98 percentage.

  • PDF

Gas-chromatographic determination of methylthiohydantoin amino acid as N(O)-butyldimethylsilyl derivatives in amino acid sequencing with methylisothiocyanate (Methylisothiocyanate를 이용한 아미노산 배열결정시 N(O)-butyldimethylsilyl 유도체로서의 methylthiohydantoin 아미노산의 기체 크로마토그래피에 의한 분석)

  • Woo, Kang-Lyung
    • Applied Biological Chemistry
    • /
    • v.35 no.2
    • /
    • pp.132-138
    • /
    • 1992
  • For effective determination of methylthiohydantoin amino acids(MTHs) by gas liquid chromatography in the protein sequencing, derivatization with N-methyl-N-(tert.-butyl-dimethylsilyl)trifluoroacetamide(MTBSTFA), a new silylating reagents, was attempted instead of trimethylsilyl(TMSi) derivatives by N,O-bis(trimethylsilyl)trifluoroacetamide(BSTFA) used up to the present and N(O)-butyldimethylsilyl MTHs derivatized by MTBSTFA were analysed on HP-1 capillary column. Twenty one protein amino acids except cystine were indentified. Especially arginine that did not detected with TMSi derivative on packed column until now was resolved by derivatization with MTBSTFA. N(O)-butyldimethylsilyl MTHs showed multiple peaks by MTBSTFA were proline, isoleucine, glycine and tyrosine and hydroxyproline especially showed several extraneous peaks more than two. Calibration curves of N(O)-butyldimethysilyl MTHs of amino acids in the range of $2.5\;nmol{\sim}7.5\;nmole$ showed good linearity. however, those of lysine, histidine and arginine showed linearity in the range of $5.0\;nmole{\sim}15.0\;nmole$. Correlation coefficients and regression coefficients of all calibration curves were highly significant(p<0.001).

  • PDF

Thermodynamic Studies on the Adsorption of 4-Octylphenol on Carboxen by GC/MS Analysis (GC/MS 분석에 의한 4-Octylphenol의 Carboxen 흡착에 대한 열역학적 연구)

  • Lee, Joon-Bae;Park, Woo-Yong;Shon, Shungkun;Jung, Ji Eun;Jeong, Yong Ae;Gong, Bokyoung;Kim, Yu-Na;Kwon, O-Seong;Paeng, Ki Jung
    • Applied Chemistry for Engineering
    • /
    • v.29 no.3
    • /
    • pp.356-361
    • /
    • 2018
  • It is common to analyze volatile organic compound (VOC) or semi-VOC (SVOC) in a sample composed of a complex matrix consisting of multiple components such as bloods through a separation process. Adsorption is a physical phenomenon in which certain components accumulate on the surface of other phases. In order to overcome difficulties in the pretreatment process, an adsorption is frequently used. Solid phase microextraction (SPME) equipment with porous carbon carboxen (CAR) is an example of adsorption application. In this study, the adsorption of 4-octylphenol to carboxen was examined. To do so, the extraction efficiency for such solvents as dichloromethane ($CH_2Cl_2$, DCM), ethylacetate ($CH_3COOC_2H_5$, EA) and diethylether ($C_2H_5OC_2H_5$, $Et_2O$) was studied and also the derivatization reaction for 4-octylphenol with reagents of bistrimethylsilyltrifluoroacetamide (BSTFA), methylchloroformate (MCF) and pentafluorobenzylbromide (PFBBr) was compared. The combination of DCM and BSTFA showed good performance thus they were adopted for this study. Thermodynamic adsorption experiments showed that the adsorption process was endothermic and Freundlich isotherm equation was more suitable than Langmuir isotherm. It was also found that the adsorption followed a pseudo-$2^{nd}$ order kinetic model.

Mesoporous Silica Catalysts Modified with Sulfonic Acid and Their Catalytic Activity on Ring Opening Polymerization of Octamethylcyclotetrasiloxane (술폰산으로 표면개질된 메조기공 실리카 촉매의 제조 및 Octamethylcyclotetrasiloxane 개환중합에서의 촉매 활성)

  • Lee, Yeonsong;Hwang, Ha Soo;Lee, Jiyoung;Lo, Nu Hoang Tien;Nguyen, Tien Giang;Lee, Donghyun;Park, In
    • Applied Chemistry for Engineering
    • /
    • v.31 no.4
    • /
    • pp.383-389
    • /
    • 2020
  • Mesoporous silica solid catalysts modified with sulfonic acid were prepared for cationic ring-opening polymerization of octamethylcyclotetrasiloxane (D4). Two sets of MCM-41 (1.7 and 2.8 nm) and SBA-15 (8.1 and 15.9 nm) with different pore sizes were used as catalyst supports. The surface of silica materials was modified with (3-mercaptopropyl)trimethoxysilane by silylation reaction and oxidized to sulfonic acid. The structures of the prepared catalysts were examined by X-ray diffraction and nitrogen adsorption-desorption. The pore size, specific surface area, and pore volume of the modified solid catalysts decreased slightly. In addition, the modification of the sulfonic acid on the silica surface was confirmed by using infrared spectroscopy and nuclear magnetic resonance spectroscopy. To observe the effect of the particle size on the catalytic activity, it was observed with a scanning electron microscope. The catalysts were used to synthesize PDMS through a ring-opening polymerization of D4, and the conversion and polymerization rate of the polymerization reaction depended on the pore size, specific surface area, particle size, and particle agglomeration of the catalysts. In order for the polymerization rate, the catalyst prepared with SBA-15 of 8.1 nm pore size had the fastest reaction rate and showed the best catalytic activity.

Structure Analysis of Water-soluble Polysaccharides Extracted from The Unripe Fruit of Cudrania tricuspidata (꾸지뽕나무 열매에서 추출한 수용성 다당류의 구조분석)

  • Kim, Seok Ju;Lee, Kyung-Tae;Youe, Won-Jae;Lee, Sung-Suk;Kim, Yong Sik
    • Journal of the Korean Wood Science and Technology
    • /
    • v.42 no.6
    • /
    • pp.740-746
    • /
    • 2014
  • The unripe fruit of cudrania tricuspidata was extracted with 50% ethanol. The crude water-soluble extracts were separated by liquid-liquid separation with n-hexane, ethyl acetate and butanol followed by precipitation with ethanol, and then the water-soluble polysaccharide (F1) was isolated by the fractionation through gel permeation chromatography using preparative PLaquagel-OH column with water. The structure was characterized by monosaccharide composition with HPAEC-PAD, methylation analysis with GC-MS, FT-IR and HPLC. According to the data, F1 was com posed of glucose (22.84 mM), galactose (13.75 mM), arabinose (45.87 mM), xylose (7.49 mM). It was revealed which uronic acid and acetyl group were not attached in F1. And it is constituted of 1-linked arabinose, 1,4-linked arabinose, 1,3-linked glucose, 1,4-linked galactose, 1,4-linked glucose, 1,3,6-linked galactose, 1,3,6-linked glucose and the ratio was showed 1.1 : 1.0 : 4.9 : 7.5 : 3.0 : 3.1 : 1.4 : 1.5.

Eritadenin Contents Analysis in Various Strains of Lentinula edodes using LC-MS/MS (LC-MS/MS를 이용한 표고 균주별 에리타데닌 함량 분석)

  • Park, Young-Ae;Lee, Kyoung-Tae;Bak, Won-Chull;Kim, Myung-Kil;Ka, Kang-Hyeon;Koo, Chung-Duck
    • The Korean Journal of Mycology
    • /
    • v.39 no.3
    • /
    • pp.239-242
    • /
    • 2011
  • Eritadenine, a potent compound of hypocholesterolemic activity, was investigated in relation to its content in domestic cultivars and wild types of shiitake (Lentinula edodes). Eighteens strains of shiitake were tested for the quantification of eritadenine by LC-MS/MS analysis. Among the strains, wild type-40 was highest as the content was 3.912 mg/g. Also, Soohyangko was 3.352mg/g, Sanlim No. 9 3.008mg/g, Chunbaegko 2.832 mg/g, Gaeulhyang and KFRI 675 both 2.792 mg/g as high-content strains. Soohyangko and Chunbaegko are applied strains for registration in 2010. Soohyangko is high-temperature type with concentrated fruiting, and 90% of production occurs in the first year, thus, recovery of cost is very fast. Chunbaegko is mid-temperature type with concentrated flushing, and produces "hwago", the best quality, in spring. Wild type-40 is excellent in productivity and is prepared for registration. Wild type-40 could be used as parent strain to make new strain with high eritadenine content.