高分子印迹固相萃取-气相色谱/质谱法测定动植物油脂中15+1种欧盟优控多环芳烃

朱琳; 阮华; 马永建; 刘华良

高分子印迹固相萃取-气相色谱/质谱法测定动植物油脂中15+1种欧盟优控多环芳烃

Determination of the 15+1 European Priority Polycyclic Aromatic Hydrocarbons in Vegetable and Animal Oil by Using Molecularly Imprinted Solid-phase Extraction Followed by Gas Chromatography-mass Spectrometry

摘要

摘要:
目的建立一种高分子印记固相萃取-气相色谱/质谱联用(MISPE-GC/MS)法测定动植物油脂中15+1种欧盟优控多环芳烃的检测方法。
方法样品经环己烷稀释后, 于高分子印记固相萃取柱净化, 洗脱液最终浓缩定容至200 μL, 采用气相色谱柱分离, 选择离子模式进行扫描, 内标法定量。
结果本方法检出限为0.25~0.94 μg/kg。对所有目标化合物在2~200n μg/L范围内有很好的相关性, 相关系数均大于0.99。日内精密度小于15%, 在2、10、20 μg/kg 3个加标水平下, 16种PAHs回收率为37.90%~105.24%, 相对标准偏差均小于15%。
结论本实验所建立的方法灵敏度好、选择性高。

Abstract:
Objectives A method based on molecularly imprinted solid-phase extraction and gas chromatography-mass spectrometry (MISPE-GC/MS) for the determination of 15+1 European priority polycyclic aromatic hydrocarbons in vegetable and animal oil has been developed.
Methods The oil samples were diluted with cyclohexane and cleansed up by molecularly imprinted solid-phase extraction catridge (MISPE). The fraction was concentrated to 200 μL for GC/MS analysis. The PAHs were separated on an Agilent J&W DB-EUPAH column(20 m×0.18 mm×0.14 μm), selected ion monitoring (SIM) mode was used and CHRD12, BaPD12 and DiPD14 were used as internal standards for quantification.
Results The detection limits of 16 PAHs were 0.25~0.86 μg/kg, The linear relation for all target compounds were in the range of 2~200 μg/L with a correlation coefficient over 0.99. The Intra-day precision is less than 15%. The recoveries of spiked samples at the level of 2, 10 and 20 μg/kg were in the rang of 37.90%~105.24%, the relative standard deviations were all less than 15%.
Conclusion The method was sensitive and selective.

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