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

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(phthalicacidesters,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。

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.