Rapid and Simple Detection of Paraquat and Diquat in Beverages Using Pipette-Tip Solid-Phase Extraction

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  • ピペットチップ型固相抽出を用いる清涼飲料水等に混入されたパラコート及びジクワットの簡易定性試験法
  • ピペットチップガタコソウ チュウシュツ オ モチイル セイリョウ インリョウスイ トウ ニ コンニュウ サレタ パラコート オヨビ ジクワット ノ カンイ テイセイ シケンホウ

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Abstract

A rapid and simple detection for paraquat (PQ) and diquat (DQ) intentionally mixed in beverages was developed. A pipette tip-type micro volume solid-phase extraction device, OMIX® pipette tip (solid-phase type ; C18, C4 and SCX) was used for the extraction of PQ and DQ. The extracted PQ and DQ were successfully detected by a color test and/or liquid chromatography/mass spectrometry (LC/MS). An 100 μL volume of a sample (coke or coffee spiked with appropriate amounts of PQ and DQ) was alkalinized by adding 100 μL of 0.1 M sodium carbonate buffer (pH 10). Then, PQ and DQ in the mixture were retained onto the C18 or C4 phase of an OMIX® pipette tip by 10-times repeating the aspirate/dispense cycles using a manual micropipettor. After being washed with water and methanol, PQ and DQ were eluted with 100 μL of 5 mM ammonium formate (pH 2.5) by 5-times repeating the aspirate/dispense cycles. It took only 3 minutes for one sample preparation. The color test was carried out by adding an 1 M sodium hydroxide solution and sodium hydrosulfite to half of the extract and the remaining part was subjected to LC/MS analysis. The extracted PQ and DQ were successfully separated and each of the [M + H] + ions were observed under the optimized LC/MS condition. The extraction procedure using an SCX-type pipette tip was more simple than the other type of solid phase. PQ and DQ were retained to the SCX phase without any adjustment of the pH and eluted with a saturated aqueous sodium chloride solution. This procedure was suitable for a color test, but not for LC/MS by because of the large amount of sodium chloride in the extract. This method was very useful for suspicious cases of PQ and DQ poisonings in beverages.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 58 (12), 1029-1034, 2009

    The Japan Society for Analytical Chemistry

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