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J Assoc Off Anal Chem. 1979 Nov;62(6):1239-46.
A simple, rapid technique is described for the determination of 2- and 3-tert-butyl-4-hydroxyanisole (BHA), tert-butylhydroquinone (TBHQ), 3,5-di-tert-butyl-4-hydroxytoluene (BHT), 2,6-di-tert-butyl-4-hydroxymethylphenol (Ionox-100), 2,4,5-trihydroxybutyrophenone (THBP), propyl gallate (PG), octyl gallate (OG), dodecyl gallate (DG), and nordihydroguaiaretic acid (NDGA) in vegetable oils, lards, and shortenings. The antioxidants are partitioned from hexane-oil into acetonitrile, concentrated under vacuum, and determined by reverse phase, gradient elution, high performance liquid chromatography with detection at 280 nm. The mobile phase is water-acetonitrile with 5% acetic acid. With this system, only Ionox-100 and OG are not resolved. Recoveries from soya-sunflower seed oil spiked at 16 and 100 ppm and from lard at 32 ppm for 8 of the 9 antioxidants ranged from 96 to 103%, 100 to 102%, and 98 to 102%, respectively. The recoveries of BHT, due to incomplete extraction, were 84, 85, and 87%, respectively.
本文描述了一种简单、快速的技术,用于测定植物油、猪油和起酥油中的2-和3-叔丁基-4-羟基茴香醚(BHA)、叔丁基对苯二酚(TBHQ)、3,5-二叔丁基-4-甲基苯酚(BHT)、2,6-二叔丁基-4-羟甲基苯酚(Ionox-100)、2,4,5-三羟基丁酰苯(THBP)、没食子酸丙酯(PG)、没食子酸辛酯(OG)、没食子酸十二酯(DG)和去甲二氢愈创木酸(NDGA)。抗氧化剂从己烷-油相中分配到乙腈中,在真空下浓缩,然后通过反相梯度洗脱高效液相色谱法在280nm波长处进行检测。流动相为含5%乙酸的水-乙腈。在该系统中,只有Ionox-100和OG无法分离。9种抗氧化剂中的8种,在大豆-葵花籽油中添加16ppm和100ppm、在猪油中添加32ppm时的回收率分别为96%至103%、100%至102%和98%至102%。由于萃取不完全,BHT的回收率分别为84%、85%和87%。