Key Laboratory of Soil Environment and Pollution Remediation, Institute of Soil Science, Chinese Academy of Sciences, Nanjing, Jiangsu 210008, China.
Chemosphere. 2013 Aug;92(8):1010-6. doi: 10.1016/j.chemosphere.2013.03.035. Epub 2013 May 6.
Risk assessment of polycyclic aromatic hydrocarbons (PAHs) contaminated soil and source apportionment require accurate analysis of the concentration of each PAH congener in the soil. However, determination of low level PAH congeners in soil is difficult because of similarity in the chemical properties of 16 PAHs and severe matrix interferences due to complex composition of soils. It is therefore imperative to develop a sensitive and accurate method for determination of low level PAHs in soil. In this work, high performance liquid chromatography equipped with fluorescence and diode-array detectors (HPLC-FLD-DAD) was used to determine the concentration of 16 PAHs in soil. The separation of the 16 PAHs was achieved by optimization of the mobile phase gradient elution program and FLD wavelength switching program. Qualitative analysis of the 16 PAHs was based on the retention time (RT) and each PAH specific spectrum obtained from DAD. In contrast, the quantitative analysis of individual PAH congeners was based on the peak areas at the specific wavelength with DAD and FLD. Under optimal conditions the detection limit was in the range 1.0-9.5 μg L(-1) for 16 PAHs with DAD and 0.01-0.1 μg L(-1) for 15 PAHs with FLD, and the RSD of PAHs was less than 5% with DAD and 3% with FLD. The spiked recoveries were in the range 61-96%, with the exception of NaP (<40%). The results show that HPLC-FLD-DAD can provide more accurate and reliable analysis of low level PAH congeners in soil samples.
多环芳烃 (PAHs) 污染土壤的风险评估和来源解析需要准确分析土壤中每种 PAH 同系物的浓度。然而，由于 16 种 PAHs 的化学性质相似，以及土壤组成复杂导致的严重基质干扰，土壤中低浓度 PAH 同系物的测定非常困难。因此，开发一种灵敏、准确的土壤中低浓度 PAHs 测定方法迫在眉睫。在本工作中，采用配备荧光和二极管阵列检测器的高效液相色谱法（HPLC-FLD-DAD）测定土壤中 16 种 PAHs 的浓度。通过优化流动相梯度洗脱程序和 FLD 波长切换程序，实现了 16 种 PAHs 的分离。16 种 PAHs 的定性分析基于从 DAD 获得的保留时间 (RT) 和每种 PAH 的特征光谱。相比之下，单个 PAH 同系物的定量分析则基于 DAD 和 FLD 在特定波长下的峰面积。在最佳条件下，16 种 PAHs 的检出限为 1.0-9.5μg L(-1)（DAD），15 种 PAHs 的检出限为 0.01-0.1μg L(-1)（FLD），DAD 的 PAHs RSD 小于 5%，FLD 的 RSD 小于 3%。加标回收率在 61%-96%之间，除了萘 (NaP)（<40%）。结果表明，HPLC-FLD-DAD 可以为土壤样品中低浓度 PAH 同系物提供更准确、可靠的分析。
