• Title/Summary/Keyword: trifluoroacetylation

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Development and comparison of convenient residue analysis for avermectin B1 in apple and soil (사과 및 토양중 avermectin B1의 간편한 잔류 분석법 개발과 비교)

  • Lee, Kang-Bong;Kim, Yong-Du;Shim, Jae-Han;Suh, Yong-Tack
    • Applied Biological Chemistry
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    • v.35 no.2
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    • pp.115-121
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    • 1992
  • Avermectin B1(abamectin) is an very effective acaricide/insecticide. Because it is applied at low rates, the resultant residue level would be quite low and this requires highly sensitive analytical method. In this study, three analytical methods for avermectin $B1_a$, were compared in view of detectability and sensitivity. The first analytical method was an HPLC method employing the fluorescence detection of avermectin. The second analytical technique to quantitate avermectin $B1_a$, and its photodegradative delta 8,9-isomer employed trifluoroacetic anhydride and 1-methylimidazole in DMF. The new method was the modification of trifluorescence method. The average recoveries of avermectin $B1_a$ for the concentration range from 1 and 10 ng/g in whole apple fruit by fluorescence method were 90.3% and 88.2% respectively. In trifluorescence method, the recoveries of the avermectin $B1_a$ and delta 8,9-isomer were 100.7% and 94.7% in concentration from 5 ng/g and 25 ng/g. The average recoveries of 5 ng and 25 ng/g in the newly modified method were 95.0, 99.0. 96.0, 92.8% in whole apple and soil respectively.

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Analysis of lipopolysaccharides of Pasteurella multocida and several Gram-negative bacteria by gas chromatography on a capillary column (Gas chromatography의 capillary column을 이용한 Pasteurella multocida 및 기타 그람음성 세균의 lipopolysaccharide 분석)

  • Ryu, Hyo-ik;Kim, Chul-joong
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.72-80
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    • 2000
  • Lipopolysaccharides (LPS) of Pasteurella multocida (P multocida) and several Gram-negative bacterial pathogens were analyzed by methanolysis, trifluoroacetylation and gas chromatography (GC) on a fused-silica capillary column. The GC analysis indicated that LPS prepared from a strain of P multocida by phenol-water (PW) or trichloroacetic acid (TCA) extraction were quite different in chemical composition. However, LPS prepared from Salmonella enteritidis by the two extraction methods were very similar. PW-LPS extracts from different Pasteurella strains of a serotype had essentially identical GC patterns. Endotoxic LPS extracted from 16 different serotypes of P multocida by PW or by phenol-chloroform-petroleum ether procedures yielded chromatograms indicating similar composition of the fatty acid moieties but minor differences in carbohydrate content. When the chemical composition of endotoxic LPS extracted from several Gram-negative bacteria (P multocida, Pasteurella hacmolytica, Haemophilus somnus, Actinobacillus ligniersii, Brucella abortus, Treponema hyodysenteriae, Escherichia coli, Bacteriodes fragilis, Salmonella abortus equi and Salmonella enteritidis) were examined, each bacteria showed a unique GC pattern. The carbohydrate constituents in LPS of various Gram-negative bacteria were quite variable not only in the O-specific polysaccharides but also in the core polysaccharides. The LPS of closely related bacteria shared more fatty acid constituents with each other than with unrelated bacteria.

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Studies on Analytical Methods for N-Methylcarbamate Residues in Crops by Spectrophotometry and Gas Liquid Chromatography (작물체중(作物體中) N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)에 관(關)한 연구(硏究))

  • Oh, Byung-Youl;Jeong, Young-Ho;Park, Young-Sun
    • Korean Journal of Environmental Agriculture
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    • v.1 no.1
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    • pp.14-21
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    • 1982
  • Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

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