• Title/Summary/Keyword: 9-fluorenylmethyl chloroformate

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Determination of Glyphosate in Whole Blood by HPLC-fluorescence Detection (HPLC 형광검출법에 의한 Glyphosate의 혈중농도 측정)

  • 이상기;김기욱;양자열;인상환;이수연
    • YAKHAK HOEJI
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    • v.45 no.4
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    • pp.347-351
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    • 2001
  • A rapid and sensitive method for the determination of glyphosate, a phosphated amino acid herbicide, in whole blood is presented. After removal of protein, the whale blood was purified by using the anion exchange resin (Dowex 1), and derivatized with 9-fluorenylmethyl chloroformate (FMCL). Derivatized glyphosate from blood sample was injected onto a Whatman partisil 10SAX column and separated with 0.1M phosphate buffer (pH 2.5) and acetonitrile (ratio=3:1). The high performance liquid chromatography-fluorescence detection gave the detection limit of 86pg and linearity of 0.9999 in the range of 0.25 $\mu$g/ml and 25 $\mu$g/ml. The recoveries of glyphosate added to the blood samples were ranged from 75.3% to 100.4% compared to the samples prepared in water. The derivatized glyphosate was stable at various acidity and temperature. This method has been successfully applied to the blood samples of lethal intoxication with the herbicide glyphosate.

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Determination of Histamine by Reverse-Phase High Performance Liquid Chromatography with Fluorescence Detection (형광검출 역상 액체크로마토그래피에 의한 Histamine의 정량)

  • Ryu, Hee-Chun;Kim, Hyung-Ryong;Kim, Sang-Hyun;Kim, Dae-Ki;Lee, Young-Mi;Kim, Hyung-Min;An, Nyeon-Hyoung;Shin, Tae-Yong
    • Analytical Science and Technology
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    • v.9 no.2
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    • pp.198-202
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    • 1996
  • A rapid and simple method for the determination of histamine by reverse-phase high performance liquid chromatography with fluorescence detection was established. 9-Fluorenylmethyl chloroformate(FMOC) was used as fluorescent derivative reagent. The optimum conditions for the derivatization such as pH, reaction time and the concentration of FMOC were investigated. Linearity of calibration curve was obtained between $0.1{\mu}g/ml$ and $0.5{\mu}g/ml$(r=0.992) and the limit of detection was $0.01{\mu}g/ml$.

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Application of FMOC-Cl for the Quantitative Determination of N-linked Oligosaccharides (FMOC 표식에 의한 Sugar Chain의 분석)

  • Kim, Dong-Hyun;Hwangbo, Sik;Chung, Gu-Yong
    • Korean Journal of Food Science and Technology
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    • v.29 no.4
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    • pp.630-634
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    • 1997
  • A fluorescence tagging agent, FMOC-Cl (9-fluorenylmethyl chloroformate) was used for the determination of 1-amino-oligosaccharide intermediates generated from glycoproteins by peptide-N $(N-acetyl-{\beta}-D-glucosaminyl)$ asparagine amidase (N-Glycanase, PNGase F). The derivatives were separated on an Amido 80 column by HPLC using a gradient system with 25 to 51% aqueous acetonitrile and monitored by a fluorometric detector. The detection limit of FMOC-amino-oligosaccharides was $0.05{\sim}1.5$ pmol with fluorometric detection at 278 nm.

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Heat Stability and Glucose-Lowering Effect of 1-Deoxynojirimycin from Silkworm (Bombyx mori) extract Powder

  • Ryu, Kang-Sun;Lee, Heui-Sam;Kim, Kee-Young;Kim, Mi-Ja;Kang, Pil-Don
    • International Journal of Industrial Entomology and Biomaterials
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    • v.27 no.2
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    • pp.277-281
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    • 2013
  • Silkworm powder, which contains 1-deoxynojirimycin (DNJ), is a promising complementary and alternative medicine (CAM) in Korea. Silkworm powder was produced from Yeonnokjam pupae at d 3 of the 5th instar at the National Academy of Agricultural Science. The powder was derivatized with 9-fluorenylmethyl chloroformate (FMOC-Cl), and the DNJ-FMOC content was measured by HPLC. We investigated the content of 1-DNJ in the silkworm powder and its glucose-lowering effect when it was treated at different temperatures. The content of 1-DNJ was the lowest at $150^{\circ}C$, while it was constant at other temperatures. The silkworm extract powder was orally administered to diabetic mice (20 mg/kg/d) for 4 wk. Water intake did not significantly change when compared with the control group (T0). The blood glucose levels significantly decreased when mice where administered silkworm powder treated at $60^{\circ}C$ (T60) compared to the control group, but no difference was observed between the groups T100 and T150. Moreover, the blood levels of TG significantly decreased compared with the control group. Based on these results, we surmise that the properties of the silkworm extract powder were stable upon heating at $100^{\circ}C$ but not at $150^{\circ}C$.