固相萃取-气相色谱-质谱法测定食用植物油中17种塑化剂  

Determination of 17 kinds of plasticizer in edible vegetable oils by solid-phase extraction and chromatography mass spectrometry

作　　者：石金娥[1,2] 刘斌 邵秋荣 齐迹 谭辉[1] 庞博[1] 陈颖 包懿 刘俊会[1] 

机构地区：[1]吉林省产品质量监督检验院,吉林长春130103 [2]吉林省食品检验所,吉林长春130103 [3]顺德出入境检验检疫局,广东顺德528303

出　　处：《中国食品卫生杂志》2015年第5期538-542,共5页Chinese Journal of Food Hygiene

摘　　要：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 The method was established for the determination of 17 kinds of plasticizer（ PAEs,incluiding DINP） in edible vegetable oils by solid phase extraction and gas chromatography mass spectrometry. Methods The PAEs in the oil samples were extracted by acetonitrile saturated with n-hexane,further purified with special solid phase extraction column,and eluted with acetone. The eluting solvent was then collected,concentrated,and directly detected with gaschromatography spectrometry（ GC-MS）. Results The linearity of PAEs was good. The detection limits of 17 PAEs were0. 01-0. 5 mg / kg. The recoveries were 76. 5%-105. 2% in low,medium and high level spiked samples. The relative standard deviations were less than 8. 0%（ n = 6）. Conclusion Compared with GB / T 21911-2008,this method was not only suitable for the detection of DINP,but also could effectively remove the interference of grease and pigment and significantly lower the detection limits. The method was simple,accurate,solvent saving and had good reproducibility.

关 键 词：植物油 塑化剂 邻苯二甲酸二异壬酯 气相色谱-质谱法 固相萃取 净化 

分 类 号：O657.63[理学—分析化学] TS227[理学—化学]