摘要
目的建立了凝胶渗透色谱净化-超高效液相色谱法(Gel permeation chromatography-Ultra performance liquid chromatography,GPC-UPLC)测定家庭烹调油烟冷凝物(Cooking oil fume condensates,COFC)中15种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的方法并对4份试样中15种多环芳烃含量进行分析。方法烹调油烟冷凝物用混合溶剂(环己烷+乙酸乙酯=1+1)溶解,凝胶渗透色谱净化,收集8~21 min净化液,净化液在200 mbar真空度40℃水浴温度浓缩至近干,1.0 ml乙腈溶解过PTFE滤膜,ZORBAX Eclipse PAH专用柱(4.6×50 mm,1.8μm)分离,乙腈和水为流动相梯度洗脱,荧光检测器检测,外标法定量。结果 15种多环芳烃在0.5~100μg/L浓度范围内与其峰面积成良好线性关系。15种多环芳烃的检出限为2~4μg/kg,3个不同加标水平平均回收率为80.2%~110.5%,相对标准偏差小于9%。4份烹调冷凝物中,15种多环芳烃总含量在4 482.8~35 043.5μg/kg,均值为18 701.9μg/kg,烹调油烟冷凝物中多环芳烃以菲为主,约占15种多环芳烃的59%,其次是荧蒽(2 626.4μg/kg)>芘(2 585.2μg/kg)>芴(1 193.5μg/kg)>萘(621.6μg/kg),强致癌物苯并(a)芘平均含量为32μg/kg(5.5~81.2μg/kg)。结论方法灵敏度高,精密度好,分析速度快;烹调油烟冷凝物中以轻质量多环芳烃(菲,荧蒽、芘、芴、萘、苊)为主,对人体有一定危害。
[Objective] To develop a method for the determination of 15 kinds of polycyclic aromatic hydrocarbons（PAHs）in cooking oil fume condensates（COFC）by gel permeation chromatography-ultra performance liquid chromatography（GPC-UPLC）,analyze the contents of 15 PAHs in 4 samples.[Methods]COFC samples were resolved by the mixed reagents（ethyl acetate＋cyclohexane=1＋1）,and purified by Gel Permeation Chromatography（GPC）. The purified solution collected between 8-21 minutes was concentrated to nearly dry at 200 mbar and 40 ℃water bath,and resolved by 1.0 ml acetonitrile to filter with PTFE. The chromatographic separation was achieved on a ZORBAX Eclipse PAH column（4.6×50 mm,1.8 μm）using a mobile phase consisting of water and acetonitrile by gradient elution. PAHs were detected by a fluorescence detector,and quantified by an external standard method.[Results]There were good linear correlation between the concentrations of 15 PAHs and their peaks areas in the range of 0.5-100 μg/L. The detection limits of PAHs were 2-4 μg/kg. The average recoveries were in the range from 80.2%-110.5%,and the RSDs were less than 9%. Among 4 COFC samples,the total contents of 15 PAHs were 4 482.8-35 043.5 μg/kg with an average of 18 701.9 μg/kg. The main PAH in COFC was phenanthrene,accounting for 59%,followed by fluoranthene（2 626.4 μg/kg）,pyrene（2 585.2 μg/kg）,fluorine（1 193.5 μg/kg）and naphthalen e（621. 6 μg/kg）. The average level of Benzo（a） pyrene was 32 μg/kg（5.5-81.2 μg/kg）.[Conclusion]The method is characterized by high sensitivity,good precision and quick analysis. The PAHs in COFC are dominated by low molecular weight（phenanthrene fluoranthene,pyrene,fluorine,naphthalene and acenaphthene）,which pose adverse health effects to employed person.
作者
何健
甘源
唐晓琴
覃梅
程莉
明智强
周春艳
HE Jian GAN Yuan TANG Xiao-qin QIN Mei CHENG Li MING Zhi-qiang ZHOU Chun-yan(Ancdysis Department of Physical and Chemical and Hygienic Toxicology, Chongqing Center of Disease Control and Prevention, Chongqing, 400042, China Chongqing Mi Zhou Lian Fa Detection Technology Limited Company, Chongqing, 400042,China)
出处
《职业与健康》
CAS
2017年第20期2774-2778,共5页
Occupation and Health
基金
2015重庆市卫生计生委医学科研项目(2015MSXM090)
关键词
烹调油烟冷凝物
多环芳烃
超高效液相色谱
凝胶渗透色谱
荧光检测器
Cooking oil fume condensates
Polycyclic aromatic hydrocarbons
Ultra performance liquid chromatography
Gel permeation chromatography
Fluorescence detector
