冷冻法结合GC-MS/MS测定植物油中抗氧化剂

Determination of 3 Antioxidants in Vegetable Oil by Freezing Method Combined with GC-MS/MS

建立一种冷冻法结合气相色谱-质谱法快速测定植物油中3种抗氧化剂(BHA、BHT、TBHQ)含量的方法。样品经甲醇涡旋振荡提取后,采用-18℃冷冻净化,选用DB-5MS毛细管色谱柱(60 m×0.25 mm×0.25μm)分离,多反应监测模式(MRM)进行测定,外标法定量。结果表明, 3种抗氧化剂在0.10~50.0μg/mL内线性关系良好,其相关系数R2均大于0.999。3种抗氧化剂在添加水平分别为1.0、5.0和50.0 mg/kg时加标回收率范围为89.19%~98.25%,相对标准偏差范围为1.22%~2.10%, BHA检出限为0.000 5 mg/kg,定量限为0.001 mg/kg, BHT、TBHQ检出限均为0.001 mg/kg,定量限为0.004 mg/kg,采用质控样品进行验证,结果在真值范围内。参加考核样品的比对结果均为满意。该方法灵敏度高,方法重复性和准确性好,适用于食用植物油中BHA、BHT、TBHQ含量的快速筛查和测定。

In order to establish a rapid, efficient and convenient method for the determination of 3 antioxidants(BHA, BHT,TBHQ) in vegetable oil, a method for the determination of 3 antioxidants in vegetable oil by freezing method combined with GC-MS/MS was developed. After being extracted by methanol vortex oscillation, the sample was purified by freezing method and a DB-5MS capillary chromatography column(60 m×0.25 mm×0.25 μm) separation, multi reaction monitoring mode(MRM) for measurement, and external standard method for quantification. The results showed that the three antioxidants ranging from 0.10 to 50.0 μg/mL had a good linear relationship with correlation coefficients R2 greater than 0.999. Relative standard deviation ranged from 1.22% to 2.10%, and spiked recovery ranged from 89.19% to 98.25%, when three types of antioxidants were added at levels of 1.0, 5.0, and 50.0 mg/kg, respectively. The detection limit and quantitative limit of BHA were 0.000 5 mg/kg and 0.001 mg/kg, respectively. Detection limit and quantitative limit of BHT and TBHQ were 0.001 mg/kg and 0.004 mg/kg, respectively. The results were verified using quality control samples, and the results were within the true value range. The comparison results of the samples participating in the assessment were all satisfied. This method had high sensitivity, good repeatability and accuracy, which was suitable for rapid screening and determination of BHA, BHT, and TBHQ content in edible vegetable oils.