Birkholz D A, Coutts R T, Hrudey S E
Enviro-Test Laboratories, Edmonton, Alberta, Canada.
J Chromatogr. 1988 Sep 30;449(1):251-60. doi: 10.1016/s0021-9673(00)94384-x.
A method is presented for the analysis of polycyclic aromatic hydrocarbons (PAHs), polycyclic aromatic sulfur heterocycles (PASHs), and basic polycyclic aromatic nitrogen heterocycles (PANHs) in fish. The analytical procedure includes Soxhlet extraction of prepared fish tissue with methylene chloride followed by gel permeation chromatography (GPC) using Bio-beads SX-3. For PAHs/PASHs, further cleanup is performed using adsorption chromatography on Florisil (5% water deactivated) and elution with hexane. For basic PANHs further cleanup of the fish extracts after GPC is achieved using liquid-liquid partitioning with 6 M hydrochloric acid and chloroform and then basifying the aqueous phase and extracting it with chloroform. Analysis of fortified fish samples was performed using capillary gas chromatography with flame ionization detection and capillary gas chromatography-mass spectrometry. Good agreement was observed for both methods of analysis when applied to fish samples fortified with PAHs, PASHs and basic PANHs at 0.1 to 1 microgram/g, suggesting that the method is effective at removing interfering biogenic compounds prior to analysis. Average recovery of PAHs/PASHs from fortified fish tissue was 87% and 70% for fish tissue fortified at 0.24-1.1 and 0.024-0.11 microgram/g, respectively. Average recovery for basic PANHs was 97% for fish fortified at 1.2-1.4 micrograms/g.
本文介绍了一种分析鱼肉中多环芳烃(PAHs)、多环芳族硫杂环化合物(PASHs)和碱性多环芳族氮杂环化合物(PANHs)的方法。分析步骤包括用二氯甲烷对制备好的鱼肉组织进行索氏提取,然后使用Bio-beads SX-3进行凝胶渗透色谱(GPC)。对于PAHs/PASHs,使用在弗罗里硅土(5%水失活)上的吸附色谱法进一步净化,并用己烷洗脱。对于碱性PANHs,在GPC之后,通过用6 M盐酸和氯仿进行液-液分配,然后将水相碱化并用氯仿萃取来进一步净化鱼肉提取物。使用带有火焰离子化检测的毛细管气相色谱法和毛细管气相色谱-质谱法对加标鱼肉样品进行分析。当应用于添加了浓度为0.1至1微克/克的PAHs、PASHs和碱性PANHs的鱼肉样品时,两种分析方法的结果吻合良好,这表明该方法在分析前有效去除了干扰性生物源化合物。对于添加了浓度为0.24 - 1.1微克/克和0.024 - 0.11微克/克的PAHs/PASHs的鱼肉组织,平均回收率分别为87%和70%。对于添加了浓度为1.2 - 1.4微克/克的碱性PANHs的鱼肉,平均回收率为97%。