SPE净化-气相色谱-三重四极杆质谱对油脂中多环芳烃的测定
Determination of 16 PAHs in edible oil by SPE and GC-MS /MS
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摘要: 采用改进的氧化铝固相萃取前处理法,结合气相-三重四极杆质谱（GC-MS/MS）技术建立了检测油脂中16种多环芳烃分析方法。样品用正己烷提取,提取液经活性氧化铝柱吸附净化,浓缩后进行GC-MS/MS测定,外标法定量。实验结果表明,16种多环芳烃物质在低质量浓度（1μg/L）的加标水平下的平均加标回收率为77.3%89.7%,高质量浓度（50μg/L）的平均加标回收率为84.2%97.2%,相对标准偏差均小于10%;其中16种物质的方法检出限（LOD）分别为0.173.01μg/L;相关系数都大于0.991。该方法具有简单、快速、准确性高、检出限低的特点,适合于油脂中多环芳烃物质检测。Abstract: A method was developed for rapid determination of 16 Polycyclic Aromatic Hydrocarbons ( PAHs) in edible oil based on an improved Alumina solid phase extraction pre-treatment method combined with the gas-a triple quadrupole mass spectrometry ( GC-MS/MS) .Edible oil was extracted with n-hexane, the supernatant was purified by activated alumina column, the purifying liquid was concentrated then determined by GC-MS/MS with external standard method.The results showed that the ranges of spiked recoveries of 16 PAHs at 1μg /L and 50μg /L were 77.3% 89.7% and 84.2% 97.2%, respectively.The relative standard deviations were below 10%.The detection limits of 16 PAHs were 0.173.01μg /kg; the correlation coefficients were larger than 0.991.This method was simple, rapid high accuracy, and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of multiple PAHs in vegetable oil.
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