QuEChERS-气相色谱-质谱法同时测定含油脂食品中16种邻苯二甲酸酯

Simultaneous determination of 16 kinds of phthalic acid esters in fatty food by QuEChERS-gas chromatography-mass spectrometry

中文关键词:  邻苯二甲酸酯  含油脂食品  QuEChERS  气相色谱-质谱法

英文关键词:phthalic acid esters  fatty food  QuEChERS  gas chromatography-mass spectrometry

中文摘要:

      目的 建立QuEChERS-气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)同时检测含油脂食品中16种邻苯二甲酸酯(phthalic acid esters, PAEs)残留量的分析方法。方法 样品用正己烷饱和的乙腈涡旋提取, 通过QuEChERS方法净化。样品在2500 r/min下涡旋2 min, 4000 r/min离心3 min后, 吸取乙腈层至已添加25 mg石墨化碳黑(graphitized carbon black, GCB)和100 mg乙二胺-N-丙基硅烷(primary secondary amine, PSA)的净化管中进行净化。采用GC-MS检测, 外标法定量。结果 16种PAEs在0.02~2.00 mg/L范围内线性关系良好, 相关系数大于0.9991。方法的检出限和定量限分别为0.10~0.30 和0.33~1.00 mg/kg。在0.2、0.5和2.0 mg/kg 3个加标水平下的平均回收率为80.2%~97.3%, 相对标准偏差不超过7.33% (n=6)。对40份市售不同种类的含油脂食品进行检测, 总体阳性检出率为17.5%。结论 本方法简便、高效且准确可靠, 适用于不同种类含油脂食品中16种PAEs的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 16 kinds of phthalic acid esters (PAEs) in fatty food by QuEChERS-gas chromatography-mass spectrometry (GC-MS). Methods Samples were extracted with acetonitrile saturated by n-hexane and purified by QuEChERS method. After the samples were whirled at 2500 r/min for 2 min and centrifuged at 4000 r/min for 3 min, the acetonitrile layer was sucked into the purification tube added with 25 mg graphitized carbon black (GCB) and 100 mg primary secondary amine (PSA) for purification. It was detected by GC-MS and quantified by external standard method. Results The 16 kinds of PAEs had good linear correlations in the concentration range of 0.02?2.00 mg/L with correlation coefficients more than 0.9991. The limits of detection and limits of quantitation were 0.10?0.30 and 0.33?1.00 mg/kg respectively. At 3 spiked levels of 0.2, 0.5 and 2.0 mg/kg the average recoveries were 80.2%?97.3%, with the relative standard deviations no more than 7.33% (n=6). Among 40 commercially available fatty foods, the overall positive detection rate was 17.5%. Conclusion This method is simple, efficient, accurate and reliable, which is suitable for the determination of 16 kinds of PAEs in various fatty food.