フォトダイオードアレイ検出器付きHPLCを用いた野菜・果物中の22農薬の多成分分析法

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概要

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• Multi residue method for determining 22 pesticides in agricultural products was examined using high performance liquid chromatograph(HPLC) with photodiode array detector(PDA). Twenty-two kinds of pesticides were divided into 3 groups. They had 0.01〜0.04μg/ml of detective limits using S/N = 3, and showed straight working curves at 3 concentrations of 0.1, 0.5, 1.0μg/ml. Except for 3 pesticides, all were eluted in the 70-140 ml fraction from gel permeation chromatography(GPC) with ethylacetate/cyclohexane (50/50 (v/v)). Chlorfluazuron, flufenoxuron, and hexaflumuron were eluted in the 65-100 ml because of their higher molecular weight. All pesticides were eluted in the 0-25 ml fraction from the mini-column including graphitized carbon black and aminopropyl with toluene / ethyl acetate (10/90 (v/v)). We used this solvent instead of toluene / acetonitrile (25/75 (v/v)). This method is following ; a sample was extracted with acetone / water (70/30 (v/v)), concentrated under reduced pressure and extracted with ethyl acetate / hexane (50/50 (v/v)). The solution was dehydrated with sodium sulfate anhydrous, concentrated under reduced pressure, dissolved in the GPC mobiled phase, and cleaned up by GPC. The fraction of pesticide was concentrated under reduced pressure, dissolved in toluene / ethyl acetate (10/90 (v/v)), cleaned up with the mini-colomn. The solution eluted was concentrated under reduced pressure, dissolved in acetonitrile, and determined with HPLC. We analyzed 9 kinds of agricultural products fortified with 22 pesticides using this method, and got approximately good recoveries in 7 kinds of them as tomato, spinach et al. The HPLC solutions of onion and orange had many peaks caused by matrix on HPLC chromatograms, and we didn't determine recoveries, when they overlapped the peaks of pesticide. We applied this method into 15 kinds of marketed agricultural products, and this method was applicable except for grapefluit. To conclude, this method was considerd to be satisfied for simultaneous method for multi pesticide residues.

• 2003-08-29

著者

• 苗床 義隆

  (独)農林水産消費技術センター岡山センター

• 原 弘幸

  (独)農林水産消費技術センター岡山センター

• 佐藤 新

  (独)農林水産消費技術センター名古屋センター

• 杉村 豊裕

  独立行政法人農林水産消費技術センター岡山センター

• 佐藤 新

  独立行政法人農林水産消費技術センター名古屋センター

• 苗床 義隆

  独立行政法人農林水産消費技術センター門司センター

• 原 弘幸

  独立行政法人農林水産消費技術センター岡山センター

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