QuEChERS-气相色谱-串联三重四极杆质谱法测定食用油中7种抗氧化剂残留

Determination of 7 kinds of antioxidant residues in edible oil by QuEChERS-gas chromatography-tandem triple quadrupole mass spectrometry

中文关键词:  抗氧化剂  气相色谱-串联质谱  QuEChERS  食用油

英文关键词:antioxidant residue  gas chromatography-tandem triple quadrupole mass spectrometry  QuEChERS  edible oil

中文摘要:

      目的 建立QuEChERS-气相色谱-串联三重四极杆质谱法检测食用油中的特丁基对苯二酚、2,6-二叔丁基-4-甲基苯酚、丁基羟基茴香醚、二丁基羟基甲苯、3,5-二叔丁基苯酚、2,4-二叔丁基苯酚和2,6-二叔丁基苯酚7种抗氧化剂残留物的方法。方法 食用油用乙腈溶液提取, 取上清液经QuEChERS净化后过有机滤膜直接上机测定, 采用HP-5MS色谱柱分离, 在电子轰击源和多反应监测模式下外标法定量。结果 该方法能有效地区分7种抗氧化剂包括其对应异构体, 目标化合物在1~300 μg/L范围内线性和峰形良好(r2≥0.99), 检出限为0.11~2.77 μg/kg, 定量限为0.36~9.23 μg/kg, 加标回收率范围为72.51%~116.33%, 相对标准偏差为0.36%~5.82% (n=8), 实际样本中2,4-二叔丁基苯酚的检出率较高。结论 该方法操作便捷准确度高, 可以有效区分叔丁基苯酚类抗氧化剂, 适用于食用油中多种抗氧化剂的高通量检测。

英文摘要:

      Objective To establish a method for determination of 7 kinds of antioxidant residues, including tert-butylhydroquinone, 2,6-di-tert-butyl-4-methylphenol, butylated hydroxyanisole, butylated hydroxytoluene, 3,5-di-tert-butylphenol, 2,4-di-tert-butylphenol, and 2,6-di-tert-butylphenol, in edible oils by QuEChERS combined with gas chromatography-tandem triple quadrupole mass spectrometry. Methods Edible oil samples were extracted with acetonitrile, and the supernatant was purified using the QuEChERS method, followed by filtration through an organic membrane for direct analysis. Separation was achieved using a HP-5MS chromatographic column, and quantification was performed using the external standard method under electron ionization and multiple reaction monitoring modes. Results The method effectively distinguished the 7 kinds of antioxidants, including their corresponding isomers. The target compounds exhibited good linearity and peak shapes within the range of 1–300 μg/L (r2≥0.99). The limits of detection ranged from 0.11 to 2.77 μg/kg, and the limits of quantification ranged from 0.36 to 9.23 μg/kg. The spiked recovery rates ranged from 72.51% to 116.33%, with relative standard deviations of 0.36% to 5.82% (n=8). Among the actual samples, 2,4-di-tert-butylphenol had a relatively high detection rate. Conclusion This method is simple, accurate, and capable of effectively distinguishing tert-butylphenol antioxidants, making it suitable for high-throughput detection of multiple antioxidants in edible oils.