• Title/Summary/Keyword: GC/MS/SIM

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Behaviour of the Soil Residues of the Acaricide-Insecticide, [$^{14}C$]Acrinathrin;I. Behaviour during Crop(Maize) Cultivation (살비살충제 [$^{14}C$Acrinathrin 토양 잔류물의 행적 규명;I. 농작물(옥수수) 재배시의 행적)

  • Lee, Jae-Koo;Kyung, Kee-Sung;Kwon, Jeong-Wook;Ahn, Ki-Chang;Jung, In-Sang
    • Korean Journal of Environmental Agriculture
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    • v.14 no.2
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    • pp.186-201
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    • 1995
  • In order to elucidate the fate of the residues of the pyrethroid acaricide-insecticide, acrinathrin in soil, maize plants were grown for one month on the specially-made pots filled with two different types of soils containing fresh and one-month-aged residues of [$^{14}C$]acrinathrin, respectively. The mineralization of [$^{14}C$]acrinathrin to $^{14}CO_2$ during the one-month period of aging and of maize cultivation amounted to $23{\sim}24%$ and $24{\sim}33%$, respectively, of the original $^{14}C$ activities. At harvest after one-month growing, the shoots and roots contained less than 0.1% and 1% of the originally applied $^{14}C$ activity, respectively, whereas the $^{14}C$ activity remaining in soil was $65{\sim}80%$ in both soils. Three degradation products with m/z 198(3-phenoxybenzaldehyde), m/z 214(3-phenoxybenzoic acid), and m/z 228(methyl 3-phenoxybenzoate) besides an unknown were identified from acetone extracts of both soils without and with maize plants after treatment of [$^{14}C$]acrinathrin, by autoradiography and GC-MS, and those with m/z 225(3-phenoxybenzaldehyde cyanohydrin) and m/z 198 (3-phenoxybenzaldehyde) from acetone extract of the Soil A treated with 50 ppm acrinathrin and grown with maize plants for 30 days were identified by mass spectrometry. These results suggested that the hydrolytic cleavage of the ester linkage adjacent to the $^{14}C$ with a cyano group, forming 3-phenoxybenzaldehyde cyanohydrin. The removal of hydrogen cyanide therefrom leads to the formation of 3-phenoxybenzaldehyde as one of the major products. The subsequent oxidation of the aldehyde to 3-phenoxybenzoic acid, followed by decarboxylation would evolve $^{14}CO_2$. Solvent extractability of the soils where maize plants were grown for 1 month and/or [$^{14}C$]acrinathrin was aged for 1 month was less than 31% of the original $^{14}C$ activity and over 95% of the total $^{14}C$ activity in soil extracts was distributed in the organic phase. Accordingly, acrinathrin turned out to be degraded rapidly in both soils and be bound to soil constituents as well, not being available to crops.

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Volatile Flavor Components of Angelica gigas Nakai by the Storage Conditions (저장조건에 따른 당귀의 정유성분 변화)

  • Choi, Sung-Hee;Kim, Hye-Jung
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.513-518
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    • 2000
  • Volatile flavor components of Angelica gigas Nakai affected by different storage time and temperature were investigated. The aroma compounds was extracted by a simultaneous distillation and extraction method using a Likens and Nickerson's apparatus. The concentrated extract was analyzed and identified by GC and GC-MS equipped polar and nonpolar column. The yields of volatile concentrates of Angelica gigas Nakai by low temperature storage were larger than those by room temperature storage. The GC patterns of the flavor components of both resembled but the peak area of each flavor compounds was little different. Main volatile flavor components of Angelica gigas Nakai by using polar column were ${\alpha}-pinene$, ${\beta}-pinene$, terpineol, farnesol, cadinene, guaiol, isolongifolene and eudesmol etc. Main volatile flavor components of Angelica gigas Nakai by using nonpolar column were camphene, ${\beta}-pinene$, elemol, eudesmol etc.

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Determination of benzene, toluene, ethylbenzene and o-xylene in bottled waters by headspace solid-phase microextraction and gas chromatography/mass spectrometry (HS-SPME-GC/MS를 이용한 먹는 샘물 중 벤젠, 톨루엔, 에칠벤젠, 자일렌의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.119-126
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    • 2011
  • Abstract: The amount of benzene, toluene, ethylbenzene, and o-xylene (BTEX) in 30 kinds of bottled waters purchased from market and 9 kinds of tap waters from home were determined using headspace solid phase microextraction (HS-SPME). The sample was stirred at 1200 RPM G for 4 min using a magnetic bar with $100\;{\mu}m$ PDMS as adsorbent for BTEX. Then it was desorbed from the fiber for 1 min at room temperature. Quantitation was achieved using standard calibration method. The limit of detection was determined as benzene 0.39 (${\pm}0.04$) ng/mL, toluene 0.08 (${\pm}0.04$) ng/mL, ethylbenzene 0.04 (${\pm}0.01$) ng/mL, and o-xylene 0.05 (${\pm}0.02$) ng/mL. Benzene and o-xylene were not detected in any samples, but toluene was detected in 11 samples, and ethylbenzene was detected just in 3 samples among 30 investigated bottled waters. The concentration range of investigated materials for toluene and o-xylene were $0.24({\pm}0.09)\sim2.95\;({\pm}0.08)\;ng/mL$, $0.08({\pm}0.06)\sim0.93({\pm}0.10)\;ng/mL$, respectively.

Comparative Evaluation of the Analytical Methods used to Determine Pesticide Residues in Milk via Dispersive Solid Phase Extraction (Dispersive Solid Phase Extraction을 사용한 우유 내 잔류농약 다성분 동시 분석법 비교연구)

  • Oh, Nam Su;Shin, Yong Kook;Lee, Ji Young;Baick, Seung Chun
    • Journal of Dairy Science and Biotechnology
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    • v.33 no.1
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    • pp.27-34
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    • 2015
  • The aim of this study was to optimize a simple, fast, and economic analytical method for the simultaneous determination of various pesticides (aldrin, p,p'-DDT, o,p'-DDT, p,p'-DDE, ${\alpha}$-endosulfan, ${\beta}$-endosulfan, dieldrin, heptachlor, permethrin, chlordane, deltamethrin, diazinon, bifenthrin, methoprene, propargite, fenpropathrin, cypermethrin, fenvalerate, and fenpropathrin) in milk by using dispersive solid phase extraction (SPE). In this study, two different extraction methods (low temperature cleanup and liquid-liquid partitioning), which were followed by a cleanup process based on dispersive-SPE, were evaluated and compared for the 19 pesticides. The results for all the pesticides were determined by gas chromatography mass spectrometry (GC/MS) with selected-ion monitoring mode, and the matrix effect of the method was evaluated. Comparison of these approaches yielded higher and more consistent recoveries of most pesticides at fortification levels of $1{\mu}g/mL$ using low-temperature fat precipitation, followed by cleanup process based on dispersive-SPE with PSA and C18 as sorbents, than other preparation process. The relative standard deviation was <20 % and the combination of this method were very effective for the cleanup.

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Pyrolytic Reaction Pathway of Dichloromethane in Excess Hydrogen (과잉수소 반응분위기에서 Dichloromethane 열분해 반응경로에 관한 연구)

  • Won, Yang-Soo
    • Applied Chemistry for Engineering
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    • v.17 no.6
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    • pp.638-643
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    • 2006
  • Pyrolytic reaction study of dichloromethane ($CH_{2}Cl_{2}$) in excess hydrogen was performed to investigate pyrolytic reaction pathways at a pressure of 1 atm with residence times of 0.3~2.0 sec in the temperature range of $525{\sim}900^{\circ}C$. A constant feed molar ratio $CH_{2}Cl_{2}$:$H_{2}$ of 4:96 was maintained through the experiment. Reagent loss and product formation were monitored by using an on-line gas chromatograph, where batch samples were analyzed by GC/MS. Complete destruction(99%) of the parent reagent was observed at temperature near $780^{\circ}C$ with residence time over 1 sec. Major products observed were $CH_{3}Cl$, $CH_{4}$, $C_{2}H_{4}$, $C_{2}H_{6}$, and HCl. Minor products included $CHClCCl_{2}$, CHClCHCl, $CH_{2}CHCl$, and $C_{2}H_{2}$. The pyrolytic reaction pathways to describe the important features of intermediate product distributions and reagent loss, based upon thermodynamic and kinetic principles, were suggested. The results of this work provided a better understanding of pyrolytic decomposition processes which occur during the pyrolysis of $CH_{2}Cl_{2}$ and similar chlorinated methanes.

Volatile Flavor Compounds of Korean Shiitake Mushroom(Lentinus edodes) (한국산 표고버섯의 휘발성 향기성분)

  • Hong, Jai-Sik;Lee, Keuk-Ro;Kim, Young-Hoi;Kim, Dong-Han;Kim, Myung-Kon;Kim, Young-Soo;Yeo, Kyu-Young
    • Korean Journal of Food Science and Technology
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    • v.20 no.4
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    • pp.606-612
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    • 1988
  • The volatile flavor compounds of fresh and dried shiitake mushrooms(Lentinus edodes) were extracted by simultaneous steam distillation-extraction apparatus, and analyzed by combined GC and GC-MS, and effects of pH on the formation of volatile compounds in fresh shiitake mushroom were investigated. Of the 29 compounds identified from fresh shiitake mushroom, the main volatile compound was 1-octen-3-ol comprising about 74.7% of the total volatiles and that in dried shiitake mushroom was 1, 2, 4-trithiolane comprising about 66.3%. With the exception of above two compounds, 3-octanone, 1-octen-3-one, 3-octanol, cis-2-octenal, n-octanol and cis-2-octenol as $C_8$ compounds were identified. Carbon disulfide, dimethyl disulfide, dimethyl trisulfide, 1-(methyl thio)-dimethyl disulfide, 1, 2, 4, 5-tetrathiane as sulfurous compounds were also identified. The formation of $C_8$ compounds in fresh shiitake mushroom during immersion was dominant in the range of pH 6.0 to 7.0, while the formation of sulfurous compounds in the range of pH 8.0 to 9.0.

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New Esterification Method for the Simulataneous Analysis of 2,4-D, Dicamba and Mecoprop in Soil Leachates by GC/MS and GC/ ECD (새로운 유도체 합성법에 의한 토양침투수중 2,4-D, dicamba 및 mecoprop의 동시 분석법에 관한 연구)

  • Hong, Moo-Ki;Lee, Hee-Duck;Park, Kun-Sang
    • Korean Journal of Environmental Agriculture
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    • v.14 no.1
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    • pp.45-54
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    • 1995
  • esters of the acid analytes were synthesized using $H_2SO_4$ as the catalyst. Efficiency of derivatization and instrumental molecular-response were compared with herbicides methylated with $BF_3-methanol$(14% W/V), $H_2SO_4-methanol$(33% V/V), and diazomethane. The molecular integrity of TFE-2,4-D, TFE-dicamba, and TFE-mecoprop, in the mixture, was confirmed by the GC/MSD method. The TFE-Esterification efficiency was maximized by adjusting the volume of $H_2SO_4$ the reaction time, and temperature. Optimal efficiency for the herbicide mixture was obtained by adding 1 ml of $H_2SO_4$ and 1 ml of TFE to the dried sample and allowing the reaction to proceed at $22^{\circ}C$ for 8 hr or using 0.5 ml $H_2SO_4$ and 1 ml of TFE at $60^{\circ}C$. For 120 min increasing the temperature and decreasing the reaction time were required for maximum esterification efficiency. The sensitivity of the GC/ECD to the TFE esters was about $2{\sim}20$ times greater than that to the methyl ester derivatives. The herbicides were extracted and esterified to TFE derivatives simultaneously from soil leachates previously spiked with the analytes. Herbicide recovery, peak resolution, and detector sensitivity were excellent without using column cleanup procedures.

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Analysis of Physicochemical Characterization and Volatiles in Pure or Refined Olive Oils (국내 유통되는 퓨어 및 정제 올리브유의 이화학적 특성 및 향기 분석)

  • Nam, Ha-Young;Lee, Ju-Woon;Hong, Jang-Hwan;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.11
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    • pp.1409-1416
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    • 2007
  • Seven selected commercial pure or refined olive oils were obtained from the market, and their physicochemical properties and volatile characterizations were investigated. Fatty acid profiles of the analyzed olive oils showed oleic $(61.2{\sim}74.7mole%)$, palmitic $(10.2{\sim}16.8mole%)$, linoleic $(9.4{\sim}18.0mole%)$, stearic $(1.9{\sim}3.0mole%)$, palmitoleic $(0.7{\sim}2.4mole%)$ and linolenic acid $(0.5{\sim}0.9mole%)$. According to Hunter#s color measurement, pure or refined olive oils showed $L^*$ value of $92.2{\sim}99.0$, $a^*$ value of $-22.2{\sim}-3.2$, and $b^*$ value of $18.5{\sim}55.0$. Their total phenol contents ranged from 1.9 to $13.3mg/100g$ while ${\alpha}-tocopherol$ content showed $7.91{\sim}13.88mg/100g$. Oxidation stability of the pure or refined olive oils were observed by Rancimat. The induction period ranged from 17.37 to 34.72 hr while their POV were $6.83{\sim}20.31meq/kg$ oil. Electronic nose and gas chromatograph-mass spectrometry with head-space solid phase microextraction were applied to identify and discriminate the volatile compounds and flavors in pure or refined olive oils, respectively.

Allelopathic Effect against Seed Germination and Seedling Growth of Picea jezoensis of Leaf Aqueous Extracts from Competition Species (경쟁 수종들의 잎 추출 수용액이 가문비나무 종자발아 및 유묘생장에 미치는 타감효과)

  • Kim, Gil Nam;Han, Sim-Hee;Shin, Soo Jeong;Kim, Du-Hyun
    • Journal of Korean Society of Forest Science
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    • v.105 no.1
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    • pp.86-92
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    • 2016
  • This study was conducted to evaluate the allelopathic effect against the regeneration of the seedling and to identify the presence of allelochemicals in Picea jezoensis natural population in Jirisan. Water-soluble extracts from leaves of different competition plants were collected to test their effects on seed germination and seedling growth of P. jezoensis. Phenolic compounds from leaves were quantified using GC/MS. The seed germination rate and seedling growth of P. jezoensis was reduced by extracts of all competition plants leaves. Monoterpenoids compound, which are generally well known in the allelochemicals has been detected in the leaf extracts. In conclusion, allelopathic chemicals of competition vegetation in P. jezoensis natural population could inhibit the seed germination and seedling growth of P. jezoensis, that is considered as a result of the lower seedling establishment.

Isolation and Identification of Antimicrobial Compound from UlGeum (Curcuma longa L.) (울금으로부터 식품부패미생물에 대한 항균성 물질의 분리 및 동정)

  • Choi, Hae-Yeon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.9
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    • pp.1202-1209
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    • 2009
  • Antimicrobial activity of UlGeum (Curcuma longa L.) was investigated. Methanol extract of dried UlGeum was fractionated to hexane, chloroform, ethyl acetate, butanol and water fraction. The antimicrobial activity of five crude fractions were examined using impregnated paper disk agar diffusion. Ethyl acetate fraction showed the highest inhibitory effect on the microorganisms such as B. subtilis, S. aureus, E. coli, L. monocytogenes and V. parahaemolyticus at 1,000 ${\mu}g$/disc. Ethyl acetate fraction was further fractionated by silica gel column and thin layer chromatography (TLC). The antimicrobial compound was isolated from their fractions and its chemical structure was identified as a 2,3-dihydrobenzofuran by GC-MS and $^1H$-NMR.