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目的建立固相萃取-气相色谱-质谱法检测植物油中17种塑化剂(包括邻苯二甲酸二异壬酯)的方法。方法采用正己烷饱和乙腈萃取,专用固相萃取柱净化,丙酮洗脱,洗脱液经浓缩后,直接用气相色谱质谱联用仪测定。结果 17种塑化剂的线性关系较好,方法检出测限范围在0.01~0.5 mg/kg,在高、中、低3个水平下进行植物油样品加标试验,平均回收率为76.5%~105.2%,相对标准偏差RSD<8.0%(n=6)。结论本研究所用方法与GB/T 21911—2008《食品中邻苯二甲酸酯的测定》比较,不仅适用于邻苯二甲酸二异壬酯(DINP)的检测,同时净化效果能有效去除油脂及色素的干扰,明显降低方法的检出限,且操作简便、溶剂用量小、重现性好。
Objective To develop a method for the determination of 17 plasticizers (including diisononyl phthalate) in vegetable oils by solid-phase extraction and gas chromatography-mass spectrometry. Methods The sample was extracted with saturated hexane of n-hexane, purified with a special solid-phase extraction cartridge and eluted with acetone. The eluate was concentrated and directly determined by gas chromatography-mass spectrometry. Results The results showed that the linear relationship between the 17 plasticizers was good. The limits of detection were within the range of 0.01 mg / kg to 0.5 mg / kg. The spiked samples were tested at high, medium and low levels with the average recovery of 76.5% 105.2%, relative standard deviation RSD <8.0% (n = 6). Conclusion Compared with GB / T 21911-2008 Determination of Phthalate in Food, the method used in this study is not only suitable for the detection of diisononyl phthalate (DINP), but also can effectively remove grease And pigment interference, significantly reduce the detection limit of the method, and the operation is simple, small amount of solvent, good reproducibility.