固相萃取-气相色谱-质谱法测定食用植物油中17种塑化剂
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(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)

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石金娥 女 高级工程师 研究方向为食品及相关产品检测 E-mail:shije351@aliyun.com通讯作者:┣┣(中)通信作者┫┫刘俊会 男 研究员 研究方向为食品安全 E-mail:yldx1988@163.com

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Determination of 17 kinds of plasticizer in edible vegetable oils by solid-phase extraction and chromatography mass spectrometry
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(Jilin Province Product Quality Supervision and Inspection,Jilin Changchun 130103,China)

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    摘要:

    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。

    Abstract:

    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 gas-chromatography spectrometry (GC-MS). Results The linearity of PAEs was good. The detection limits of 17 PAEs were 0.01-0.5 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.

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石金娥,刘斌,邵秋荣,齐迹,谭辉,庞博,陈颖,包懿,刘俊会.固相萃取-气相色谱-质谱法测定食用植物油中17种塑化剂[J].中国食品卫生杂志,2015,27(5):538-542.

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  • 收稿日期:2015-05-27
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  • 在线发布日期: 2015-11-03
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