• Title/Summary/Keyword: capillary column

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Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Captan, Folpet, Captafol 및 Chlorothalonil의 잔류분석법)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.29 no.2
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    • pp.165-175
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    • 2010
  • A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

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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Separation properties of 209 PCB congeners on capillary columns and identification of PCBs congeners in aroclor standards for source identification (오염원 해석을 위한 폴리염화비페닐류(PCBs) 209 이성체의 컬럼별 분리 특성과 Aroclor 표준품의 이성체 확인)

  • Kim, Kyoung-Soo;Kim, Kyeo-Keun;Kim, Jong-Guk
    • Analytical Science and Technology
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    • v.19 no.4
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    • pp.352-364
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    • 2006
  • This study was performed to search for useful separation properties and elution orders of three GC columns (DB-1, DB-5MS, SPB-Octyl) for 209 PCBs congeners using M-1668A-0.01X-SET of the AccuStandard Inc.. In addition, to confirm the quantitative peak in peak pattern method, the IUPAC Nos. of PCBs congener peaks were identified with 4 Aroclor standards (Aroclor-1242, 1248, 1254 and 1260). The separation property of dioxin-like PCBs congeners by four columns (DB-1, DB-5MS, SP-2331 and SPB-Octyl) was excellent in SP-2331. DB-1 and SPB-Octyl columns are necessary to use with a column of other types.

Studies on the Analysis of Tobacco Leaf Alkaloids (잎담배 Alkaloid분석에 관한 연구)

  • 장기철;한상빈;김용옥;이운철
    • Journal of the Korean Society of Tobacco Science
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    • v.13 no.2
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    • pp.20-26
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    • 1991
  • This study was carried out to develop the method of alkaloids analysis and investigate the kinds and contents of alkaloids in flue-cured, burley and oriental tobacco leaves using developed analytical method. The developed analytical method of alkaloids was as followed : Tobacco sample was treated with acid(pH 2∼3) and extracted with chloroform to remove chemical components except alkaloids. Sample solution was treated with alkali(pH 12∼ 13) and was extracted with chloroform to obtain alkaloids from sample solution. After extraction of alkaloids from tobacco leaves, alkaloids were separated and identified by GC, GC/MS using SE-54 fused silica capillary column. Nicotine, nornicotine, myosmine, 9-nicotyline, anabasine, anatabine, 2, 3-bipyridyl, cotinine, formyl nornicotine, acetyl nornicotine and formal anatabine were isolated and identified from the extracts of tobacco leaves. The contents of alkaloids were burley > flue-cured > oriental tobacco leaves, but oriental tobacco leaves were higher nornicotine, cotinine, formyl nornicotine and acetyl nornicotine contents than those of flue-cured tobacco leaves. The burley tobacco harvested in Korea was higher nornicotine contents by 2-6 times in the portions of cutter, leaf and tips position than that of burley tobacco(B3F) harvested in V. S. A.

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Antimutagenic effects of 4-decanol identified from mustard leaf (갓으로부터 분리, 동정된 4-decanol의 항돌연변이 효과)

  • Kim, Jeong-Ok;Kim, Mu-Nam;Park, Kun-Young;Moon, Suk-Hee;Ha, Yeong-Lae;Rhee, Suk-Hee
    • Applied Biological Chemistry
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    • v.36 no.6
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    • pp.424-427
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    • 1993
  • The chloroform extract of mustard leaves (Brassica juncea Cosson) reduced mutagenicity of $AFB_1$ in bacterial assay (Salmonella typhimurium TA100). 4-Decanol was one of major compounds in the chloroform extract when analyzed by GC-MS on HP-5 capillary column. The authentic compound of 4-decanol dissolved in DMSO (0.5%) inhibited mutagenic activities of $AFB_1$ and MNNG in Salmonella typhimurium TA100 at a rate of 99% and 93%, respectively. This result indicates that 4-decanol is an antimutagenic compound present in chloroform extract of mustard leaves.

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Enantiomeric Separation of Methamphetamine Abused in Korea (우리나라에서 남용되는 메스암페타민의 거울상 이성질체분리)

  • Yoo, Young-Chan;Chung, Hee-Sun;Choi, Hwa-Kyung;Kim, Eun-Mi;Kim, Mi-Kyung;Kim, Sun-Choon
    • YAKHAK HOEJI
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    • v.41 no.3
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    • pp.277-282
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    • 1997
  • Methamphetamine, which is the most commonly abused drug in Korea, exists in terms of d-, l- isomers and a racemate(dl). d-Methamphetamine is a potent central nervous system stimulant, whereas l-Methamphetamine is sold freely as a nasal decongestant. In addition, methamphetamine appears in different ratios of optical isomers by the clandestine synthesis applied. In this study, enetiomeric separation of methamphetamines was estabilished to distinguish the chirality of methamphetamines trafficked and abused in Korea. A gas chromatograph/mass spectrometer(GC/MS) system equipped with an achiral capillary column is used to isolate the isomers of methamphetamine after (S)-N-(trifluoroacetyl)-l-prolyl(TFP) deravatization.After analyzing 10 illicit methamphetamine powders and 10 positive urine samples, following findings were found: d-Methamphetamine was well resolved from l-Methamphetamine by chromatographic separation of TFP derivatibes on DB-5 with retention time of 11.80 and 11.35 min respectively. The detection of d-Methamphetamine in all 10 powders and 10 urine samples proves that all methamphetamines abused in Korea are illegally manyfactured and administred.

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A Survey on the Droplet Generators and Principle of Droplet Generation (액적 발생기의 종류 및 액적 발생 원리에 대한 고찰)

  • Park, Bong-Yeop;Han, Jae-Seob;Kim, Seon-Jin;Kim, Yoo
    • Journal of the Korean Society of Propulsion Engineers
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    • v.4 no.2
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    • pp.54-60
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    • 2000
  • Most droplet generators are based on the Rayleigh's theory of droplet breakup, and various kind of droplet generation devices have been designed in accordance with vibrating method of capillary liquid column. At present, VOAG(Vibrating Orifice Monodisperse Aerosol Generator) is used to generate primary aerosol standards. For the combustion experiments with isolated single droplet, it is found that dripping method or separating method of suspended drop at an end of filament are more effective. Single drops can be separated from continuous streams of droplets by controlling electric charge.

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Analysis of Aromatic Acids in Panax Ginseng by Gas Chromatography (GC에 의한 인삼 중의 방향족 산성 성분 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Kim, Kyoung-Ho;Han, Sang-Bum;Han, Byung-Hoon
    • YAKHAK HOEJI
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    • v.38 no.4
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    • pp.389-393
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    • 1994
  • Eight aromatic acids in Panax ginseng were determined by GC. Ultra-1 $(25\;m{\times}0.2\;mm{\times}0.33\;{\mu}M)$ capillary column was employed with temperature programming from $150^{\circ}C$ to $240^{\circ}C$ at a rate of $3^{\circ}C/min$. The mean contents of eight aromatic acids in 8 white ginseng samples were as follows; salicylic acid: 4.30 ppm, cinnamic acid: 18.2 ppm, vanillic acid: 4.22 ppm, gentisic acid: trace, syringic acid: 6.69 ppm, p-coumaric acid: 13.3 ppm, ferulic acid : 21.9 ppm, caffeic acid: 24.3 ppm, respectively.

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Studies on the Essential Oil of Korean Valerian Root (Valeriana fauriei var. dasycarpa Hara) (한국산 쥐오줌풀(Vaieriana fauriei var. dasycarpa Hara)의 정유성분에 관한 연구)

  • 김용태;박준영;김영회;김근수;장희진;권영주;이종철;최영현
    • Journal of the Korean Society of Tobacco Science
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    • v.14 no.1
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    • pp.66-78
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    • 1992
  • The essential oil of Korean valerian root ( Valeriana fauriei roar. dasycarpa Hara) was isolated by simultaneous distillation Sl extraction. The oil content of fresh root was 0.7% (wb) and that of dried root was 2.1 5 (db) and sensory analysis of the oil indicated sweet-balsamic, woody and floral characteristic aroma notes. The oil was fractionated into one hydrocarbon fraction and three oxygenated hydrocarbon fractions by using silica gel column chromatograpy. Each fraction was analyzed by capillary GC and GC-MS. Out of 81 characterized compounds, the major compounds were a-pinene, camphene, $\beta$-pinene, bornyl acetate, borneol , bornyl iso-valerate and sesquiphellandrene and the characteristic floral and woody aroma of neutral fraction of Korean valerian root could be due to be the presence of oxygenated compounds such as borneol, bornyl acetate, bornyl iso-valerate, p-ionone ana $\beta$-ionone epoxide. Comparing the yield of Korean valerian root with those from other origins reported, oil content of Korean valerian root was higher than those of European and Indian origins.

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