二阶导数恒能量同步荧光法快速测定海产品中的苯并(a)芘

Rapid Determination of Benzo(a)pyrene in Seafood by Second-derivative Constant-energy Synchronous Fluorescence Spectrometry

摘要:

海产品中的多环芳烃主要来自于水体污染，而苯并(a)芘是公认的多环芳烃指标，本文针对海产品中的苯并(a)芘含量的检测，建立了简单快速的海产品中的苯并(a)芘含量的二阶导数恒能量同步荧光检测法。海产品样品经过微波辅助皂化萃取后，正己烷萃取液被旋蒸干，后再溶解于二氯甲烷溶液中，以二阶导数恒能量同步荧光光谱法检测，设定恒能量差为1400 cm-1，扫描范围为300~500 nm，对其中的苯并(a)芘进行快速检测，根据海产品样品的谱图特性，用负峰-基线法读荧光强度值，连续标准加入法进行定量分析，整个光谱扫描所需时间只需1 min。对实际样品检测回收率在80.5%~118.2%之间，检测限为0.10 μg/kg，定量限为0.34 μg/kg，线性范围为0.34~250 μg/kg。对海产品样品的荧光检测结果与HPLC-FL检测结果基本一致，对有证多环芳烃标准物质的检测结果与参考值一致。

Abstract:

Polycyclic aromatic hydrocarbons (PAHs) in seafood samples were ascribed to water pollution, while benzo(a)pyrene was recognized as an indicator of PAHs. A simple and rapid analytical method was developed by combining microwave-assisted pretreatment with second-derivative constant-energy synchronous fluorescence scanning technique for the determination of the benzo(a)pyrene content in seafood samples. The samples were firstly processed with microwave pretreatment, and the extractions were vaporized and redissolved into dichloromethane for further detection. According to the specific spectral properties of seafood samples, peak-to-derivative baseline measurement was used to read the fluorescence data, and standard addition method was applied to the quantitative analysis of seafood samples. The whole spectroscopic scan cost only 1 min. The recoveries ranged from 80.5% to 118.2% for seafood samples and the detection limit was 0.10 μg/kg with linear range from 0.34 to 250 μg/kg. The results obtained with this method were in consistence with those of HPLC-FL method. The satisfactory results acquired by using this method to analyze a certified reference material with a relative error of 7.1% from the certified benzo(a)pyrene concentration.