• Title/Summary/Keyword: pentafluorobenzyl bromide

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A Micro-quantification of Abscisic Acid from Plant Tissue by Pentafluorobenzyl Esterification Using GLC (Pentafluorobenzyl ester 화(化)에 의(依)한 미량(微量) Abscisic Acid 의 GLC 분석법(分析法))

  • Jeong, Young-Ho;Hong, Moo-Ki;Song, Byung-Hun
    • Korean Journal of Environmental Agriculture
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    • v.4 no.2
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    • pp.114-117
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    • 1985
  • A new method for micro-quantification of abscisic acid from plant tissue is described. GLC-ECD method of abscisic acid pertafluorobenzyl ester synthesized by reaction of plant extract with pentafluorobenzyl bromide showed higher sensitivity than that of abscisic acid methyl ester, and the detection limit of abscisic acid by the described method was as low as 5 pg.

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A case study on the fire victim in the vehicle by GC/MS through derivatization of cyanide with pentafluorobenzyl bromide (PFBBr) (시안화이온의 pentafluorobenzyl bromide (PFBBr)에 의한 유도체화 후 GC/MS 분석에 의한 차량화재 변사체 사인규명에 관한 사례연구)

  • Lee, Joon-Bae;Shon, Sung Kun;Woo, Sang Hee;Park, Se Yeon;Hwang, Jung Ho;Kwon, O-Seong;Kim, Nam Yi;Paeng, Ki Jung
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.73-78
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    • 2016
  • Hydrogen cyanide (HCN) is an extremely toxic gas frequently produced during the incineration of plastics, such as acrylonitrile-butadiene-styrene (ABS). A victim of a fire who has inhaled smoke could have cyanide in the blood. Therefore, cyanide could be a good marker for a post-mortem examination of a fire as well as carboxyhemoglobine (COHb) test of blood samples. For a particular fire case, a burned body with a suicide note was found inside a burned vehicle. Even though the COHb value is conclusive evidence, measuring the COHb for denatured blood might be difficult due to severe thermal denaturation or the formation of methemoglobin (MetHb). To overcome this difficulty, cyanide could be used as an indicator when investigating the death of a fire victim. In this study, gas chromatography/mass spectrometry (GC/MS) was adopted to measure the levels of cyanide in the blood through derivatization with pentafluorobenzyl bromide (PFBBr) under cation surfactant by scan and SIM mode. The concentration of cyanide in the blood of heart blood and brain of the victim was found to be 0.36 µg/mL and 1.20 µg/mL respectively, which was higher than the average value (0.041 µg/mL) found in the blood of 14 people who smoked.

Validation of an analytical method for cyanide determination in blood, urine, lung, and skin tissues of rats using gas chromatography mass spectrometry (GC-MS)

  • Shin, Min-Chul;Kwon, Young Sang;Kim, Jong-Hwan;Hwang, Kyunghwa;Seo, Jong-Su
    • Analytical Science and Technology
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    • v.32 no.3
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    • pp.88-95
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    • 2019
  • This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

Derivatization and Residual Determination of MCPP in Soil Leachate (토양 침투수중 MCPP의 유도체화 및 잔류분석)

  • Hong, Moo-Ki;Smith, Albert E.
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.199-208
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    • 1994
  • Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

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