食品添加物であるヨーカビーンCを試験した結果, ラウリルトリメチルアンモニウムと2, 4, 5-トリクロルフェノールがイオン結合した化合物で, 1/2分子あるいは1分子の結晶水を有する結晶であることがわかった. また, その試験法を確立するための資料を得た.

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It has been already known that dehydroacetic acid (DHA) produced a chelate compound with ferric salts. The colour developed by this reaction was stable, and the reaction was so sensitive that could be utilized as a colorimetric method for determining DHA.
A aqueous solution containing 0.5-3.5mg of DHA was transferred into a 25-ml flask, added 5ml of 2% iron alum solution, and diluted to the mark with water. The resulting solution was mixed thoroughly, the absorbances of the solution was determined at the wavelength of 440mμ.
Sorbic acid, salicylic acid, methylnaphthoquinone, nitrofurazone, nitrofurylacrylamide, acids, alkalis or colouring matters interfered with the method. Benzoic acid and esters of p-hydroxybenzoic acid did not interfere with this method in the concentration below 50mg per 100ml. However, these interferring substances could be eliminated by the steam distillation method described in the second report.

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It has been reported already that dehydroacetic acid reacted with ferric iron to produce a chelate compound. The reaction was so sensitive and quantitative that it was utilized for the colorimetric determination of dehydroacetic acid.
Suitable amount of the distillate from foods, which was made by the steam distillation method reported on Shokuhin Eiseigaku Zashi, 5, 148 (1965), was transferred into a 25-ml flask, added with 5ml of iron alum solution and diluted to the mark with water. The absorbance of the solution was measured at 440mμ. More than 10μg/ml of dehydroacetic acid in the distillate could be determined by this method. Sorbic acid and salicylic acid interfered with this method, but other food preservatives did not interfere within the regular amount. Nitrofurazone, nitrofurylacrylamide, artificial sweetners and coloured substances did not appear in the distillate.

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Benzoic acid in foodstuffs has been detected by various chromatography, and the identification of small amounts of benzoic acid is possible. The acid has been determined ultraviolet spectrophotometrically, or volumetrically. However, the determination of the acid is disturbed by other acidic substances.
In the present report, studies on the infrared spectrometric analysis of the acid are described. The results obtained are as follows:
1. Characteristic absorption of benzoic acid in carbon tetrachloride in IR-region provides an infrared spectrometric method of analysis of the acid.
2. 1690cm^-1 are useful as key band for the quantitative analysis of the acid.
3. The interfering effects of other food additives on this method have been investigated, and the analysis of benzoic acid was found to be possible, except sorbic acid.
4. This method and ultraviolet spectrophotometry were applied to the market foods, and both measured values were found nearly equal.

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In general, dehydroacetic acid in foodstuffs has been determined by ultraviolet spectrophotometry, or colorimetry with salicylaldehyde.
In the present report, studies on the infrared spectrometric analysis of the acid are described.
The results obtained are as follows:
1. Characteristic absorption of dehydroacetic acid in carbon tetrachloride in IR-region provides an infrared spectrometric method of analysis of the acid.
2. Carbonyl band 1, 750cm^-1 are useful as key band for the quantitative analysis of the acid.
3. The interfering effects of other food additives on this method have been investigated, and the detection of the acid was found to be possible, but its determination was found to be difficult.

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1) Nitrofurazone (NF) 0.1%添加飼料その他によるラット飼育実験を行ない, 睾丸障害作用につき病理組織学的に検索しつぎの成績を得た.
2) NF投与により, 精細胞系のうち精子, 精子細胞および第二次精母細胞にまず変性壊死を起こすが, 精祖細胞は次第に侵されて数を減らしながらも長期間残存し分裂能を保持する. セルトリ細胞は変性しない. 間質では間細胞の増殖が, 精細管基底膜には軽度の肥厚が3か月飼育例で認められたが, この変化は続発的なものである.
3) ラット睾丸に組織学的に障害を与えるNF最低添加濃度は0.06%であり, これは1日当り約50mg/kgの摂取に相当する.
4) NF 0.1%添加飼料投与で3日間飼育により睾丸精細胞に変性が起こる.
5) 睾丸の精子形成機能の障害は, 実験の範囲では可逆性で, 0.1%で1か月投与の場合約60日でほぼ尋常に回復した. なお, 回復に要する時間は, 投与期間の長短に著しく左右されることがない.
6) 実験成績を総括して, 現在の法定添加量では, ほぼ安全性に危険はないものと考えられる.

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以上食品添加物公定書に準用して炭酸塩の検査を行なうとほとんどすべての製品がこの項目だけで不合格となる.
硫酸カルシウムは, 豆腐用のほか, 食品添加物中カルシウム剤の原料としても用途が多く, 公定書集載の純度試験法で判定を下すには問題がある.

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ガスクロマトグラフィーが出現したとき, 農薬分析への応用についてもいち早く試みられたが, これまでに述べたように残留分析への応用に実用化されたのはMC-D, EC-Dが開発されてからであった. EC-Dは最近国産品が作製され, ようやく発売される段階に立ち至った. 今までは有機塩素剤には適確な化学反応がなかったため, わが国では農作物中の残留分析に関するデータは皆無に等しかった. 今後, EC-D, MC-D自体についてもさらに改良が加えられるであろうが, 分析技術者に課せられた命題はclean up, カラムの選択および分離能の理論的解明等であろう. さらに有機塩素化合物の植物または動物体内における代謝, あるいは日光による分解産物の同定, 分離等まだ未解決の問題が多く残されている. 今後EC-Dが国内において普及し, 大いにその有用性が期待されるときにあたり, 米国その他の国々における実情を調査し, それを総括して紹介した次第である.

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