超高效液相色谱法测定橄榄油中8种受阻酚类抗氧化剂及迁移研究

Determination of 8 hindered phenolic antioxidantsin olive oil by ultra-performance liquid chromatography and its migration research

目的建立橄榄油中没食子酸丙酯（PG）、叔丁基对苯二酚（TBHQ）、去甲二氢化愈创木酸（NDGA）、叔丁基对羟基茴香醚（BHA）、3，5-二叔丁基-4-羟基苄醇（Ionox100）、没食子酸辛酯（OG）、没食子酸月桂酯（DG）和2，6-二叔丁基对甲酚（BHT）等8种受阻酚类抗氧化剂的超高效液相色谱检测方法；研究食品模拟溶剂中受阻酚类抗氧化剂迁移量的迁移规律。方法采用乙腈提取，C18填料基质分散固相萃取，超高效液相色谱检测；在20、60和100℃三个模拟温度下测定PG、BHA和BHT从聚乙烯膜中迁移至橄榄油、20％乙醇、10％乙醇和3％乙酸4种模拟溶剂的量。结果8种物质的保留时间小于8．5min，无需衍生化，检测限为0．01～0．05μg／mL，线性相关系数（R^2）均大于0．999，方法的平均回收率为80．0％-106．8％，精密度（RSD）为0．69％～7．94％。对PG、BHA和BHT进行常规加热迁移实验，随着浸泡时间的延长迁移量增加，PG在水性食品模拟溶剂中的迁移量和橄榄油中的迁移量差别不大；BHA、BHT易溶于油脂中，在橄榄油中的迁移量最大，在其他模拟溶剂中，随着乙醇含量的减少，BHA和BHT的迁移量较少，BHA在20％乙醇中的迁移量大于10％乙醇和3％乙酸。结论受阻酚类抗氧化剂随着温度的升高迁移量增大，易迁移至脂肪模拟溶剂中。

Objective To develop a method for determination of PG, TBHQ, NDGA, BHA, Ionoxl00, OG, DG and BHT in olive oil by ultra-performance liquid chromatography （UPLC）, and to study the migration rule of hindered phenolic antioxidants in food simulation solvent. Methods The samples were extracted with acetonitrile, and C1s dispersion matrix solid-phase, the separation were performed by UPLC. The migration amount of PG, BHA, BHT from polyethylene film to different simulated solvent （olive oil, 20% ethanol, 10% ethanol, 3% acetic acid） were determined at 20,60 and 100 %. Results The retention time of 8 hindered phenolic antioxidants was less than 8.5 rain. The limits of detection were in the range of 0.01 - 0.05 txg/mL, and the linear correlations were 〉 O. 999. The average recoveries were from 80.0% to 106.8% , and the relative standard deviations were between 0.69% and 7.94%. The original heating migration experiments of PG, BHA and BHT were performed by such method. As the extension of heating time, the migration amounts were increased, and the migration amounts of PG in water-based food simulation solvent was similar in olive oil. BHA and BHT easily migrated to simulate fat solvents. The migration amount was the maximum in olive oil, while the migration amounts of BHA and BHT were little as the ethanol decreased in other simulation solvents. The migration amount of BHA in 20% ethanol was more than in 10% ethanol and 3% acetic acid. Conclusion With the increase of temperature, the migration amount increase, and the hindered phenolic antioxidants easily migrate to simulate fat solvents.