Detection of Phthalic Acid Esters from Sodium Sulfate and Organic Solvents Used for Pesticide Residue Analysis

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  • Yoshikawa Noriko
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University
  • Umino Yukiko
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University
  • Obata Miki
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University
  • Sakagawa Rie
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University
  • Semma Masanori
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University
  • Ito Yoshio
    Faculty of Pharmaceutical Sciences, Mukogawa Women's University

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  • 残留農薬分析に用いる無水硫酸ナトリウム及び有機溶剤からのフタル酸エステルの検出
  • ザンリュウ ノウヤク ブンセキ ニ モチイル ムスイ リュウサン ナトリウム オヨビ ユウキ ヨウザイ カラ ノ フタルサン エステル ノ ケンシュツ

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Abstract

In the analyses of pesticide residue by GC-MS (CI), it was very occasionally observed that unidentified peaks appeared from sample solutions. After preliminary investigations, these peaks were identified as phthalic acid esters (PAEs). PAEs including DBP (Di-n-butyl phthalate), DEHP (Di-2-ethylhexyl phthalate) and DEP (Diethyl phthalate) were shown to be contained in organic solvents with high purity of pesticide residue analysis grade. The highest level of total PAEs was detected in n-hexane (0.0237μg/mL), followed by acetonitrile (0.0139μg/mL), dichloromethane (0.0117μg/mL), ethyl acetate (0.0084μg/mL) and diethyl ether (0.0083μg/mL). These 3 PAEs were also detected in eluate from 11 samples of anhydrous sodium sulfate (Na2SO4) purified for PAEs determination grade, pesticide residue analysis grade, fluorescent analysis grade, etc., packed in glass columns with above organic solvents. As using dichloromethane for elution from different grade of Na2SO4, the highest level of total PAEs (4.13μg/g) was eluted from one of pesticide residue analysis grade, followed by PAEs determintation grade (1.75μg/g) and one of laboratory grade (1.51μg/g). In all of these 3 samples of Na2SO4, more than about 90% of total PAEs was detected in the 1st fraction (after 2 hrs, 40mL).

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