抽出浮選/吸光光度法による血清中の亜鉛の定量(<特集>超微量分析のための前処理と予備濃縮)

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書誌事項

タイトル別名
  • Extraction flotation/spectrophotometric determination of zinc in serum.
  • 抽出浮選／吸光光度法による血清中の亜鉛の定量
  • チュウシュツ フセン キュウコウ コウドホウ ニ ヨル ケッセイチュウ ノ ア

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抄録

A spectrophotometric method for the determination of Zn in serum, based on the extraction flotation of 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino) phenol (5-Br-PAPS)-Zn(II) chelate with the aid of tetrahexylammonium chloride (THA) as a collector and small nitrogen bubbles, has been developed. Only 0.1 ml of sample was necessary, because preconcentration for Zn in serum was carried out by the use of extraction flotation technique. Interference of Fe and Cu in serum could be removed by the masking action of 2, 2'-bipyridyl and salicylaldoxime, respectively. The recommended procedure is as follows. Serum (50 to 100 μl) mixed with 0.1 ml of 1 M hydrochloric acid was heated at 8095°C for 2 min. After cooling, 0.1 ml of trichloroacetic acid (0.05 g ml-1) solution was added, the mixture was shaken and centrifuged, and the supernatant solution was removed. Then, the precipitated proteins were washed two times with 0.5 ml each of water. To the combined supernatant solution, 1 ml of ascorbic acid (0.01 g ml-1) solution, 1 ml of 5 × 10-3 M 2, 2'-bipyridyl solution, 1 ml of 5-Br-PAPS (80μg ml-1) solution and 5 ml of 0.2 M carbonate buffer solution (pH 8.9) were added. After standing for 15 min, 1 ml of THA (0.008 g ml-1) solution was added and diluted to 20 ml with water. The solution (pH 8.79.1) was placed in a flotation cell with 0.7 ml of isopentyl alcohol-butyl acetate (2:1 in vol.). After bubbling nitrogen through the aqueous phase at 40 ml min-1 for 5 min, the organic phase was removed and make up to 1 ml with 0.2 ml of salicylaldoxime (0.01 g ml-1) ethanolic solution and ethanol, and its absorbance was measured at 556 nm. Zinc(II) was collected as 5-Br-PAPS-Zn (II) chelate with about 98% yield in the mixed solvent solution. Results were in good agreement with those of AAS method. Moreover, hemoglobin did not interfere at a concentration up to 0.3 mg hemoglobin ml-1 in serum.

収録刊行物

  • 分析化学

    分析化学 36 (11), 745-749, 1987

    公益社団法人 日本分析化学会

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