• Title/Summary/Keyword: Selected ion monitoring(SIM)

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Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Quantitative Comparison of Radiation-induced 2-Alkylcyclobutanones from Irradiated Beef and Chicken (쇠고기와 닭고기로부터 방사선 조사에 의해 유도된 2-Alkylcyclobutanone류의 정량적 비교 분석)

  • Kim, Kyong-Su;Kim, Eun-Ah;Lee, Hae-Jung;Park, Eun-Ryeong;Yang, Jae-Seung;Byun, Myung-Woo;Kim, Sun-Min;Lee, Myung-Yul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1495-1502
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    • 1999
  • Gamma-irradiated beef and chicken at the dose levels of 0.5 to 10 kGy were subjected to the detection of radiation-induced 2-alkylcyclobutanones whether irradiated or not. Radiation-induced 2-alkylcyclobutanones were extracted from beef and chicken fats, separated by florisil column chromatography and identified with GC/MS method by selected ion monitoring(SIM). When beef and chicken were irradiated, 2-dodecylcyclobutanone, 2-tetradecylcyclobutanone and 2-(5'-tetradecenyl)cyclobutanone were formed from palmitic, stearic and oleic acids. Concentrations of 2-alkylcyclobutanones were linearly increased with the dose levels of irradiation and depended upon the composition of fatty acids in beef and chicken. Radiation-induced 2-alkylcyclobutanones in irradiated beef and chicken were remarkably detected at 1 kGy and over, while these compounds were not detected in non-irradiated samples. The concentrations of radiationinduced 2-alkylcyclobutanones were relatively constant during 6 months.

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Plant Growth Promotion Activity of Endophytic Fungi Isolated from the Roots of Calystegia soldanella (갯메꽃 뿌리로부터 분리된 내생진균의 식물생장촉진활성)

  • You, Young-Hyun;Yoon, Hyeok-Jun;Woo, Ju-Ri;Seo, Yeong-Gyo;Shin, Jae-Ho;Choo, Yeon-Sik;Lee, In-Jung;Kim, Jong-Guk
    • Microbiology and Biotechnology Letters
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    • v.39 no.4
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    • pp.324-329
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    • 2011
  • Eight endophytic fungal strains were isolated from the roots of Calystegia soldanella from the western coast of South Korea. The culture filtrate of the eight endophytic fungi were applied to waito-c rice seedlings in order to verify potential plant growth promotion activities. The results of bioassay indicated that the Cs-9-7 fungal strain possessed the highest plant growth promotion activity. Fungal culture filtrates were analyzed to verify secondary metabolites using gas chromatography and mass spectroscopy with selected ion monitoring (GC/MS-SIM). The culture filtrate of the Cs-9-7 fungal strain was confirmed to contain gibberellins GA3 (1.229 ng/mL), GA4 (3.535 ng/mL), GA7 (1.408 ng/mL) and GA12 (0.378 ng/mL). Polymerase chain reactions (PCR) were performed so as to determine the internal transcribed spacer (ITS) regions for the identification of isolated strains with universal primers ITS-1 and ITS-4. The Cs-9-7 fungal strain, isolated from the root of C. soldanella, has been named Aspergillus tubingensis Cs-9-7.

Plant growth-promoting activity and identification of endophytic fungi isolated from native plant in East coast (동해안 자생식물로부터 분리된 내생균류의 식물생장촉진활성 및 동정)

  • You, Young-Hyun;Jin, Yong Ju;Kang, Sang-Mo;Oh, Sejong;Lee, Myung-Chul;Kim, Jong-Guk
    • Korean Journal of Microbiology
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    • v.51 no.1
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    • pp.14-20
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    • 2015
  • Coastal plant species, Plantago camtschatica Cham. native to the coastal region of the East Sea were sampled and then morphologically different 20 endophytic fungal strains were purely isolated. Phylogenetic analysis of isolates was done by the Bayesian program based on sequenced internal transcribed spacer (ITS-rDNA) region. Culture filtrates of each of 20 isolates were treated to Waito-c rice (WR) seedlings for verifying plant growth-promoting activity, respectively. As the results, E/PC/10/1 strain showed the highest plant growth-promoting activity among them. The culture filtrate of the strain E/PC/10/1 was revealed as containing gibberellins ($GA_1$, $GA_3$, $GA_4$) by using HPLC, and gas GC/MS with selected ion monitoring (SIM). Finally, this strain was identified as novel Penicillium spinulosum species that producing new GAs with microscopic observation and further molecular analysis with beta-tubulin gene sequence.

High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Gibberellin A4 Producted by Fusarium solani Isolated from the Roots of Suaeda japonica Makino (칠면초의 뿌리로부터 분리된 Fusarium solani에 의해 생산된 지베렐린 A4)

  • Seo, Yeonggyo;You, Young-Hyun;Yoon, Hyeokjun;Kang, Sang-Mo;Kim, Hyun;Kim, Miae;Kim, Changmu;Lee, In-Jung;Kim, Jong-Guk
    • Journal of Life Science
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    • v.22 no.12
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    • pp.1718-1723
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    • 2012
  • Ten endophytic fungi with different colony morphologies were isolated from the roots of Suaeda japonica Makino growing naturally in Suncheon Bay. Plant growth promotion was verified by treating waito-c rice seedlings with culture filtrates from the endophytic fungi. The bioassays showed that the Sj/7/4 fungal strain induced effective growth promotion in the seedlings. The gibberellins (GA) produced by fungal strain Sj/7/4 were analyzed by gas chromatography /mass spectroscopy with selected ion monitoring (GC/MS SIM). The culture filtrate of Sj/7/4 fungal strain was confirmed to contain $GA_4$ through quantitative analysis. The Sj/7/4 fungal strain was identified to determine the internal transcribed spacer (ITS) regions with universal primers ITS-1 and ITS-4 by using polymerase chain reactions (PCR). Molecular analysis of the Sj/7/4 fungal strain showed high similarity to Fusarium solani. The Sj/7/4 fungal strain isolated from the root of S. japonica was therefore designated as F. solani Sj/7/4.

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea (국내 미등록 제초제 cyanazine의 농산물 중 개별 잔류분석법 개발)

  • Choung, Myoung-Gun;Im, Moo-Hyeog
    • Journal of the Korean Society of International Agriculture
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    • v.30 no.4
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    • pp.339-346
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    • 2018
  • Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

Analysis of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol by Solid Phase Extraction (고체상 추출에 의한 1,3-dichloro-2-propanol과 3-chloro-1,2-propanediol의 분석)

  • Chae, Hee-Jeong;In, Man-Jin;Kim, Min-Hong;Han, Keum-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.1
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    • pp.183-187
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    • 1997
  • The analytical conditions of 1,3-dichloro-2-propanol (DCP) and 3-chloro-1,2-propanediol (MCPD) by solid phase extraction were optimized to improve recovery. Selected-ion monitoring technique which was used for GC-MS analysis of both compounds gave substantially higher sensitivity. The detection limits of DCP and MCPD were 25 and 50 ppb, respectively. The effects of extraction column type, elution solvent and salt concentration on recovery were examined. A normal phase column was better than a reverse phase column in solid phase extraction of DCP and MCPD. It was explained in terms of polarity relationship of solvent-solute-solid phase. A maximum recovery was obtained at the salt concentration of 20% (w/v). Water-immiscible and chloropropanol-soluble solvents such as chloroform, diethyl ether, hexane and ethyl acetate were tested for elution solvent. Hexane and ethyl acetate were the most suitable solvents for the extraction of DCP and MCPD, respectively. High recovery better than 95% was obtained with the selected solvents.

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Migration of di-(ethylhexyl)phthalate from PVC food packaging materials detected plasticizer into flood simulanting solvent (가소제가 검출된 PCV 식품용기에서의 식품유사침출 용매에 따른 디에틸헥실프탈레이트 용출에 관한 연구)

  • 김일영;유인실;이정미;김성단;정소영;한상운
    • Proceedings of the Korean Society of Food Hygiene and Safety Conference
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    • 2002.05a
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    • pp.127-131
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    • 2002
  • Migration of di-(ethylhexyl)phthalate (DEHF) from PVC food packaging materials detected plasticizer into food simulanting solvents(4% Acetic acid, 8% Ethanol, 50% Ethanol, 95% Ethanol, Heptane) were studied. For executing this study ,2 PVC food packaging materials detected DEHP were used. Analysis was by GC-FID and GC-MSD(selected ion monitoring) for DEHP, and optimized for quantification of plasticizer. The recovery of DEHP into food simulanting solvents were min. 87.4${\pm}$ 3.6 ∼ max. 109.9 ${\pm}$ 10.7% respectively. Following exposure to food simulants 95% Ethanol for 24hours at 60$^{\circ}C$ the migration results of 1020.90 ${\pm}$ 10.15$\mu\textrm{g}$/g, 563.54 ${\pm}$ 5.60$\mu\textrm{g}$/dm$^2$and 73.51 ${\pm}$ 5.09$\mu\textrm{g}$/g 149.22 ${\pm}$ 10.34$\mu\textrm{g}$/dm$^2$were detected from the container for lunch and for stock fish respectively.

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