高效液相色谱-荧光检测法测定水产品中15种多环芳烃

Determination of 15 polycyclic aromatic hydrocarbons in aquatic products by HPLC-Fluorescence

    摘要
  • 摘要: 建立了高效液相色谱荧光检测法同时测定水产品中15种多环芳烃(polycyclic aromatic hydrocarbons，PAHs)的方法。通过液相色谱柱、荧光激发和发射波长等条件的优化，实现了15种多环芳烃组分基线完全分离和荧光高灵敏度检测。在优化的试验条件下，检测的15种多环芳烃中萘、苊和芴的检出限为0.5 μg · kg-1，苯并b荧蒽、二苯并a, h蒽和苯并g, h, i苝的检出限为2.0 μg · kg-1，其余化合物的检出限为1.0 μg · kg-1；在检测的15种多环芳烃中，菲、蒽、芘、苯并a蒽、崫、苯并a芘、茚并1,2,3-cd芘在0.001~0.500 mg · L-1质量浓度范围，其余化合物在0.002~1.000 mg · L-1质量浓度范围，呈良好的线性相关，相关系数R2>0.995；样品加标水平分别为2.0 μg · kg-1、10.0 μg · kg-1和100.0 μg · kg-1时回收率为71.1%~98.4%，相对标准偏差(RSD) < 10%。该检测方法重现性高，检测灵敏度和准确度均满足分析要求。

     

    Abstract: We used high performance liquid chromatography (HPLC) coupled to a fluorescence detector (FLD) to determine 15 polycyclic aromatic hydrocarbons (PAHs) in aquatic products and realized complete base-line separation of the 15 PAHs and high sensitive fluorescence determination based on optimization of liquid chromatographic conditions, excitation and emission wavelength. Under optimizing conditions, the detection limit of naphthalene, acenaphthene and fluorene is 0.5 μg · kg-1; that of benzo (b) fluoranthene, dibenzo (a, h) anthracene and benzo (g, h, i) perylene is 2.0 μg · kg-1; that of the others is 1.0 μg · kg-1. PHE, AN, PY, BaA, CHR, BaP and IP are in the range of 0.001~0.500 mg · L-1, and the others are in the range of 0.002~1.000 mg · L-1, having good linearity (R2>0.995). The recovery at the spiked amount of 2.0 μg · kg-1, 10.0 μg · kg-1 and 100.0 μg · kg-1 is 71.1%~98.4% (RSD < 10%). The reproducible, sensitive and accurate method is suitable for quality control of the 15 PAHs in aquatic products.

     

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