• Title/Summary/Keyword: 액체크로마토그래피-텐덤질량분석기법

Search Result 2, Processing Time 0.014 seconds

Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
    • /
    • v.22 no.11
    • /
    • pp.1456-1462
    • /
    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Distribution and Risk Assessment of Perfluorinated Compounds (PFCs) in Major Drinking Water Treatment Plants, Korea (국내 주요 정수장의 과불화화합물 분포 및 위해성 평가)

  • Son, Boyoung;Lee, Leenae;Yang, Mihee;Park, Sangmin;Pyo, Heesoo;Lee, Wonsuk;Park, Juhyun
    • Journal of Korean Society of Water and Wastewater
    • /
    • v.31 no.6
    • /
    • pp.491-499
    • /
    • 2017
  • The chemical structures of perfluorinated compounds(PFCs) have unique properties such as thermal and chemical stability that make them useful components in a wide variety of consumer and industrial products. Two of these PFCs, perfluorooctane sulfonate(PFOS) and perfluorooctanoic acid(PFOA), have received attention and were the most commonly detected. In this study it was analyzed the concentrations of 8 PFCs in samples were collected from drinking water treatment plants for 5 years(2012-2016). PFOS and PFOA were also high concentration and frequency. The mean concentrations of PFOA and PFOS were detected $0.0026-0.0069{\mu}g/L$ and $0.0009-0.0024{\mu}g/L$ in samples from drinking water treatment plants. These were relatively lower or similar compared to PFOS concentrations in Osaka(Japan). In general, these levels are below health-based values set by international authoritative bodies for drinking water. These results will be serve as the first monitoring data for PFCs in drinking water and be useful for characterizing the concentration distribution and management of PFCs in future studies.