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目的建立肉制品中12种多环芳烃化合物的气相色谱-质谱(GC/MS)同时测定方法。方法样品经搅碎混匀后,称取一定量经正己烷-丙酮溶液(体积比为1∶1)超声波提取,提取液经中性氧化铝小柱净化,以正己烷-二氯甲烷溶液(体积比为1∶1)洗脱后浓缩,正己烷定容后,用气相色谱-质谱法分离测定。结果本法在0.1μg/ml~5.0μg/ml时有良好的线性关系,相关系数为0.996 7~0.999 9,仪器检出限为0.04 ng/ml~45 ng/ml,除二苯并(a,h)蒽的定量限为49μg/kg外,其余PAHs的定量限为0.04μg/kg~3.9μg/kg。结论利用超声提取、中性氧化铝小柱净化、气相色谱法分离、质谱法检测建立的肉制品中12种多环芳烃化合物的同时测定方法具有简单、易操作、准确度和重现性好的特点。
Objective To establish a simultaneous determination of 12 polycyclic aromatic hydrocarbons (PAHs) in meat products by gas chromatography-mass spectrometry (GC / MS). Methods Samples were crushed and mixed, then weighed a certain amount of n-hexane - acetone solution (volume ratio of 1: 1) ultrasonic extraction, the extract was neutral alumina column purification, n-hexane - dichloromethane solution Volume ratio of 1: 1) eluted and concentrated, n-hexane after volume, by gas chromatography - mass spectrometry separation and determination. Results The method showed a good linearity in the range of 0.1μg / ml ~ 5.0μg / ml, the correlation coefficient was 0.996 7 ~ 0.999 9, the detection limit was 0.04 ng / ml ~ 45 ng / ml. , h) The limit of quantification for anthracene is 49 μg / kg. The limits of quantification for other PAHs range from 0.04 μg / kg to 3.9 μg / kg. Conclusion Simultaneous determination of 12 polycyclic aromatic hydrocarbons (PAHs) in meat products by ultrasonic extraction, neutral alumina cartridge purification, gas chromatography separation and mass spectrometry was simple, easy to operate, accurate and reproducible Features.