分散式固相萃取结合高效液相色谱法快速测定 油脂中三种抗氧化剂含量

Determination of 3 antioxidant residues in edible oil by high performance liquid chromatography with dispersive solid phase extraction

中文关键词:  高效液相色谱法  分散固相萃取  抗氧化剂  食用油脂

英文关键词:high performance liquid chromatography  dispersive solid phase extraction  antioxidants  edible oil

中文摘要:

      目的 建立食用油脂中叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、特丁基对苯二酚(TBHQ)残留的快速检测方法。方法 采用分散式固相萃取技术结合高效液相色谱(HPLC), 选用中性氧化铝作为吸附剂, 以整合了吸附剂活化、目标物提取和样品净化等步骤的“一步式”前处理方式净化样品, 最后用高效液相色谱二极管阵列检测器(DAD)对三种抗氧化剂含量进行测定。结果 在优化实验条件下, 方法的线性范围为0.2 ~200 mg/L, 线性相关系数R2≥0.9997, 对BHA、BHT、TBHQ的检出限(S/N=3)均为0.5 mg/kg, 回收率为85.5%~95.4%, 峰面积的相对标准偏差为2.10%~3.53%。结论 本文所建立的方法较液液萃取、固相萃取、凝胶渗透色谱等传统的方法更为简便快速, 高效环保, 成本低廉, 可满足油脂中BHA、BHT、TBHQ含量检测需求; 整个样品前处理过程仅需10~15 min, 适合BHA、BHT、TBHQ含量检测的批量实验。

英文摘要:

      Objective An analytical method for the determination of BHA, BHT and TBHQ residues in edible oil was investigated. Methods The new method based on dispersive solid phase extraction coupled with high performance liquid chromatography (HPLC) was established. Using Alumia-N as adsorbent, the traditional adsorbent activation, sample cleaning and target extraction were integrated as the “one-step” sample preparation process. Then the three antioxidants were analyzed by HPLC (Diode array detector, DAD). Results Under the optimized condition, using HPLC-DAD, the calibration of antioxidants were linear in the range of 0.2~200 mg/L with R2 more than 0.9997. In addition, the limit of detection (LOD) was found of 0.5 mg/kg (S/N=3). The spiked recoveries of the BHA, BHT and TBHQ from animal and plant oil were in the range of 85.5%~95.4%, with the relative standard deviations (RSDs) of peak area of 2.10%~3.53%. Conclusion Compared to the traditional methods such as liquid-liquid extraction, solid phase extraction and gel permeation chromatography (GPC), this method was easy, quick, good efficient, low-pollution and low-cost. It only took 10~15 min, suitable for batch experiments.