高效液相色谱-荧光检测法测定贝类中15种多环芳烃

Determination of 15 Polycyclic Aromatic Hydrocarbons in Shellfish by HPLC- FLD

建立了高效液相色谱-程序荧光检测法同时测定贝类中15种多环芳烃的方法。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。在优化的实验条件下，检测的15种多环芳烃中萘、苊和芴的检出限为0.5μg/kg，苯并[b]荧蒽、二苯并[a，h]蒽和苯并[g，h，i]苝的检出限为2.0μg/kg，其余化合物的检出限为1.0μg/kg；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0.001～0.5 mg/L浓度范围，其余化合物在0.002～1.0 mg/L浓度范围，呈良好的线性相关，相关系数r＞0.995；当样品加标水平分别为2、10、100μg/kg时，回收率在71.1％～98.4％， 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。

High performance liquid chromatography （ HPLC） coupled to a fluorescence detector （ FLD） was used to set up an analytical procedure for the quantification of 15 EU priority polycyclic aromatic hydrocarbons （ PAHs） in aquatic products.The method realized the complete base -line separation of 15 PAHs and high sensitive flurescence determination after optimizing analytical conditions , including liquid chromatographic conditions , excitation and emission wavelength.Under the optimized conditions , the detection limits of naphthalene , acenaphthene and fluorene were 0.5 μg/kg, the detection limits of benzo（b）fluoranthene, dibenzo（a,h）anthracene and benzo（g,h,i）perylene were 2.0 μg/kg, the detection limits of the others were 1.0 μg/kg.The 15 PAHs had good linearity （ r〉0.995 ） , in the range of 0.001～0.5 mg/L.The recoveries at the spiked amount of 2, 10, and 100μg/kg, respectively, were 71.1%～98.4%, and the RSDs were less than 10%.The method is highly sensitive and accurate.It can be used for the quality control of 15 PAHs in many aquatic products.