リン酸アルキルアンモニウムを添加した移動相を用いる逆相高速液体クロマトグラフィーによるヨウ化物イオン及びヨウ素化チロニン類の同時分析  [in Japanese] Simultaneous Determination of Iodide and Iodothyronines by Reversed-Phase High-Performance Liquid Chromatography with an Alkylammonium Phosphate-Containing Mobile Phase  [in Japanese]

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Abstract

イオン対(IP)試薬としてリン酸アルキルアンモニウムを添加した移動相を用いる紫外吸光(UV)検出/逆相高速液体クロマトグラフィー(HPLC)で,ヨウ化物イオン(I<sup>-</sup>)及びヨウ素化チロニン類を同時分析する方法を検討した.本研究では,カラムにSunrise C18を用い,移動相の諸条件(pH,IP試薬の種類など)がI<sup>-</sup>及びヨウ素チロニン類の保持に及ぼす影響を系統的に調べた.その結果から,分離に至適な移動相として5 mMリン酸トリブチルアンモニウム(pH 3.0)-アセトニトリル(64 : 36, v/v)を選定し,これらのヨウ素化合物を分析した.いずれの化合物も良好な定量性を示した.この分析法を市販の甲状腺ホルモン製剤に含まれるI<sup>-</sup>及びヨウ素化チロニン類の同時分析に応用した.

We developed a novel reversed-phase high-performance liquid chromatographic (RP-HPLC) method with a mobile phase containing an alkylammonium phosphate as an ion-pairing reagent for the simultaneous determination of iodide (I<sup>−</sup>) and iodothyronines {thyronine (T0), triiodothyronine (T3), reverse triiodothyronine (rT3) and thyroxine (T4)}. The iodo compounds were chromatographed on a Sunrise C18 column (150 × 4.6 mm I.D.) at a flow-rate of 1.0 mL min<sup>−1</sup> with UV detection at 225 nm and 10-μL injection. We investigated the influence of the mobile-phase parameters, which were the pH, the concentration of an ion-pairing reagent, the concentration of an organic modifier and the type of ion-pairing reagent, for the retention of iodo compounds. Good RP-HPLC separation of the iodo compounds was achieved using a mobile phase of 5 mM tributylammonium phosphate (pH 3.0)-acetonitrile (64 : 36, v/v). The calibration curves for I<sup>−</sup>, T0, T3, rT3 and T4 were linear over concentration ranges of 5.0 × 10<sup>−7</sup> − 5.0 × 10<sup>−4</sup>, 2.5 × 10<sup>−7</sup> − 2.5 × 10<sup>−4</sup>, 2.0 × 10<sup>−7</sup> − 2.0 × 10<sup>−4</sup>, 2.0 × 10<sup>−7</sup> − 2.0 × 10<sup>−4</sup> and 2.0 × 10<sup>−7</sup> − 2.0 × 10<sup>−4</sup> M, respectively. The detection limits (<i>S/N</i> = 3) for I<sup>−</sup>, T0. T3, rT3 and T4 were 2.6 × 10<sup>−8</sup>, 4.0 × 10<sup>−8</sup>, 1.2 × 10<sup>−8</sup>, 1.4 × 10<sup>−8</sup> and 1.3 × 10<sup>−8</sup> M, respectively. We applied this method for the simultaneous determination of I<sup>−</sup> and iodothyronines in commercial thyroid tablets.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 60(2), 149-156, 2011-02-05

    The Japan Society for Analytical Chemistry

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Codes

  • NII Article ID (NAID)
    10027410153
  • NII NACSIS-CAT ID (NCID)
    AN00222633
  • Text Lang
    JPN
  • Article Type
    ART
  • ISSN
    05251931
  • NDL Article ID
    11009203
  • NDL Source Classification
    ZP4(科学技術--化学・化学工業--分析化学)
  • NDL Call No.
    Z17-9
  • Data Source
    CJP  NDL  J-STAGE 
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