旋涡振荡萃取- 超高效液相色谱法检测脂肪食品模拟物橄榄油中6 种抗氧化剂

为建立高效且易于操作的脂肪食品模拟物橄榄油中抗氧化剂双酚A(BPA)、叔丁基对羟基茴香醚(BHA)、3,5- 二叔丁基-4- 羟基苯甲醇(Ionox100)、2,6- 二叔丁基对甲酚(BHT)、2,4,6- 三叔丁基苯酚(TTBP)、2,2′- 亚甲基双(4- 乙基-6 叔丁基酚)(AO425)的测定方法，采用旋涡振荡甲醇萃取- 旋转蒸发浓缩以及旋涡振荡乙酸乙酯- 环己烷(1:1，V/V)萃取- 凝胶渗透色谱(GPC)净化浓缩两种前处理方法进行处理，采用超高效液相色谱法(UPLC)检测。结果表明：本方法具有较低的检出限(LODs 分别为0.06、0.04、0.01、0.03、0.06、0.01mg/L)、较好的线性(R2 ＞0.998)、较高的回收率(两种前处理方法平均回收率分别高于83.0%、56.8%)及较高的精密度(RSD 分别小于7.5%、8.4%)。将该方法用于食用油样品的检测，结果显示，只有BHT 被检测出，且含量低于其特定迁移限量(SML)。

Vortex-mixing Extraction and Ultra Performance Liquid Chromatography for the Analysis of 6 Antioxidants in Fatty Food Simulant Olive Oil

An efficient and simple analytical method has been developed for the determination of 6 phenolic antioxidants, namely 4,4＇isopropylidendiphenol (BPA), tert-butyl-4-hydroxyanisole (BHA), 2,6-di-tert-butyl-4-hydroxy-methylphenol (Ionox100), 2,6-di-tert-butyl-p-cresol (BHT), 2,4,6-tri-tert-butylphenol (TTBP) and 2,2 ＇-methylenebis-(6-tert-butyl-4-ethylphenol) (AO 425) in fatty food simulant olive oil. Two methods, namely extraction with methanol on a vortex mixer followed by concentration using a rotary evaporator (hereinafter referred to as Method 1) and extraction with cyclohexane/ethyl acetate mixture (1:1, V/V) on a vortex mixer followed by gel permeation chromatographic concentration (hereinafter referred to as Method 2) were separately used for sample pretreatment before ultra performance liquid chromatographic (UPLC) analysis. The merits of figure of the developed method were as follows: respective limits of detection (LODs) for BPA, BHA, Ionox100, BHT, TTBP and AO 425, 0.06, 0.04, 0.01, 0.03, 0.06 mg/L and 0.01 mg/L; correlation coefficients of calibration curve of the analytes, larger than 0.998, indicating good linearity; and respective average spike recoveries for the analytes in samples pretreated by Methods 1 and 2, larger than 83.0% and 56.8%, with RSDs of smaller than 7.5% and 8.4%. This method was used to determine some commercial edible oils from different plants, and only BHT was detected in all of them, the contents of which were all much lower than the Chinese national specific migration limit.