• Title/Summary/Keyword: Capillary column gas chromatography

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Protein Hydrolysis with Formic Acid and Analysis of Amino Acid Using Butylthiocarbamyl - trimethylsilyl (BTC - TMS) Derivatives by Gas Chromatography

  • 우강융;이동선;김민철
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.3
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    • pp.320-324
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    • 2003
  • The protein hydrolysis with 6 M formic acid containing 0.3% tryptamine was a superior method for amino acid analysis of standard amino acid and protein than 6 M HCI containing 0.3% tryptamine. The recoveries of standard amino acid after acid hydrolysis were more accurate in the 6 M formic acid hydrolysis than 6 M HCI hydrolysis, especially recovery of tryptophan showed higher values of 1.5 times than that of 6 M HCI hydrolysis. The results of analysis on the standard protein, bovine serum albumin, showed very similar values compared to the sequence analysis reported in the literature for the 6 M formic acid hydrolysis than 6 M HCI hydrolysis, especially in the tryptophan recovery as standard amino acid recovery. Butylthiocarbamyl - trimethylsilyl (BTC - TMS) derivatives of 22 standard amino acids were successfully resolved DB-17 capillary column. Excellent reproducibility of standard amino acid recovery and composition of bovine serum albumin were obtained with BTC-TMS derivatives.

Studies on the Simultaneous Determination of VNA and TSNA by GC - TEA (Gas chromatography-Thermal Energy Analyzer에 의한 휘발성 니트로소아민과 담배 특유의 니트로소아민들의 동시 분석연구)

  • Rhee, Mun-Su;Ji, Sang-Woon;Park, Yang-Su
    • Journal of the Korean Society of Tobacco Science
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    • v.15 no.2
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    • pp.174-184
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    • 1993
  • This is to investigate the methodology for the simultaneous determination of Wk, mk and TSNA using gas chromatography(GC) in combination with chemiluminescence detector, thermal energy analyzer(TEA) . The simultaneous analysis has been estimated by evaluating tobacco. The TEA was linked to GC equipped with non -polar SPB -5 fused silica capillary column which was introduced into the ceramic pyrolysis tube by the point of 16cm from the end of TEA. Quantification was carried out by internal standardization with WDPA after calibration of retention times and response factors with authentic nitrosoamines. It was demonstrated that WDPA was most preferable as internal standard for the simultaneous analysis. The recoveries of the internal standard were in the range of 83∼96% . Nitrosoamines in this method were detected with determination limit of 0.1ng and was made by a straight line in calibration curve by TEA response. The suitability of nitrosoamines extraction in tobacco leaf was investigated. It was most suitable to extract nitrosoamines from tobacco leaves with 0.01 M NaOH within a period of 8 hours. Thimerosal as an antibacterial agent was added to NaOH solution to prevent artifactual formation. The fractionation and the purification of nitrosoamines form alkaline extracts were conveniently performed using Extrelut multilayer column and dichloromethane. Reproducible and reliable results were obtained for the determination of nitrosamines in a relatively short time compared to previous known method. TSNA contents in burley were about 4 times higher as those in the fluecured tobacco.

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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
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    • v.24 no.2
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    • pp.171-176
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    • 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.

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Analysis of Sterols and Its Hydrogenation to Stanols in Vegetable Oils for the Development of a Cholesterol Absorption-lowering Neutraceutical (콜레스테롤 흡수저하 기능성소재 개발을 위한 식물성 유지 중이 Sterols 분석 및 Stanol로의 수소첨가반응)

  • 인만진;김동청;채희정;김명희;임병순;김의용
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.5
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    • pp.980-983
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    • 1999
  • The contents of sterols and stanols in vegetable oils and mist oil were analyzed by gas chromatography using a capillary column. The total sterol contents showed high values of 0.67~0.89g/100g in corn oil, rice bran oil, red pepper seed oil and sesame oil. Mist oil, a byproduct of soybean oil manufacture, was a suitable raw material for the production of stanol since it showed high sterol content (10.2g/100g). In the hydrogenation of sterol contained in mist oil using Pd catalyst, the effects saponification of oil were examined. The conversion of sterol to stanol was improved by a factor of 4~5 through saponification of oil, compared to the reaction without saponification.

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기체크로마토그래피-질량분석검출기와 고체상미량추출법을 이용한 물 중의 MTBE 미량분석

  • Jeon Chi-Wan;Lee Jeong-Hwa;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.195-198
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    • 2005
  • A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.

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Studies on the Phenol Compounds in Smoke Total Particulate Matters of Flue-cured Tobacco Leaves (황색종 잎담배의 연기응축물중 페놀 화합물에 관한 연구)

  • 복진영;백순옥;김상범;안동명;조수헌
    • Journal of the Korean Society of Tobacco Science
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    • v.23 no.2
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    • pp.162-167
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    • 2001
  • This study was carried out to quantitatively determine phenol compounds in smoke total particulate matter(TPM) to evaluate the qualititive characteristics of flue-cured tobacco varieties(NC82, KFl14 and KFl18). After collecting The TPM by using smoking machine, the concentration of phenol compounds were analyzed by gas chromatography as their trimethylsilyl derivative on a fused capillary column bonded with a 5% PE ME siloxane stationary phase. In all the flue-cured tobacco varieties, the major phenol components were monohydroxy compounds. The order of the highest concentration of total phenol compounds in TPM was NC82, KF114 and KFl18 but the contents of dihydroxy compound in the KFl18 was higher than those of NC82 and KF114.

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Solid-Phase Extraction of L-Muscone from Aqueous Samples with Amberlite XAD-4 for Gas Chromatographic Assay

  • Paik, Man-Jeong;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.27 no.5
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    • pp.539-543
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    • 2004
  • An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the co-extracted interferences. The overall method showed excellent linearity ($r^2{\geq}$ 0.9994) in the range of 0.1 to 2.0 $\mu\textrm{g}$/mL with good intra- and inter-day precisions (% RSD = 2.5~7.3) and with high extraction recovery rates ($\geq$ 98.1 %). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 $\mu\textrm{g}$/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD $\leq$ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.

A Study on Capillary Gas-Liquid Chromatographic Determination of Diosgenin in Costus Speciosus (모세관 기체-액체 크로마토그래피에 의한 Costus Speciosus 중 Diosgenin의 정량에 관한 연구)

  • Taek Jae Kim;Cha Kee Surk;Kim Young Sang
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.369-376
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    • 1986
  • Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

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A Study on the Simultaneous Analysis of Regulated Pesticides Residues from Rice and Soy Bean (쌀과 콩 중 규제잔류 농약의 동시분석에 관한 연구)

  • Taek-Jae Kim;Yun-Woo Eo;Jae-Seong Rhee
    • Journal of the Korean Chemical Society
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    • v.35 no.5
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    • pp.560-568
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    • 1991
  • The simultaneous determination method which simply determined regulated pesticides was investigated. Sample was extracted with acetone-methanol and partitioned with methylene chloride after addition of saturated NaCl solution. Entract was purified by Bio-Beads S-X3 column using cyclohexane-methylene chloride (1 : 1) as eluate. The determination of pesticides was performed by BP-1 capillary column gas chromatography using ECD and NPD. The average recoveries of pesticides in rice and soy fbean were over 83% and 81%, respectively. It was possible to detect pesticides in rice up to 0.002 ppm by $\alpha-BHC$ and up to 0.05 ppm by carbaryl and in soy bean up to 0.01 ppm by ${\alpha}$-BHC and up to 0.3 ppm by carbaryl.

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Gas Chromatography Residue Analysis of Bifenthrin in Pears Treated with 2% Wettable Powder

  • Choi, Jeong-Heui;Liu, Xue;Kim, Hee-Kwon;Shim, Jae-Han
    • Toxicological Research
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    • v.25 no.1
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    • pp.41-45
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    • 2009
  • This study was conducted to monitor the level of bifenthrin residues in pear sprayed with 2% bifenthrin wettable powder (WP) at the recommended rate at four different schedules prior to harvest. The target analyte was extracted with acetone, partitioned into dichloromethane, and then purified by florisil chromatographic column. The residue determination was performed on a DB-5 capillary column using GC with electron capture detector (ECD). Linearity of this method was quite good ($r^2$ = 0.9951) in the concentration ranged from 0.2 mg/kg to 10 mg/kg. Recovery test was carried out at two concentration levels, 0.2 mg/kg and 1.0 mg/kg, in three replicates, and their rates were from 82.9% to 107.2%. No quantitative bifenthrin was detected in pear of all kinds of treatments including the treatment sprayed 4 times until 7 days before harvest. This sensitive and selective method can be used to monitor the trace residual amounts of bifenthrin in pear in a quite low concentration level.