UPLC-DAD-FLD测定土壤中多环芳烃

本文建立了以加速溶剂萃取（ASE）和固相萃取为提取和净化手段，采用超速液相色谱-二极管阵列-荧光检测器（UPLC-DAD-FLD）串联捡测土壤中16种多环芳烃的方法。通过色谱柱的比较，选择更小粒径和内径的分析柱（Supelco SILTMLC．PAH，100×3．0mm，3μm），缩短了分析时间，也节省了溶剂（乙腈），满足大量样品的快速灵敏分析的需要。在保留时间定性的基础上，利用PDA获取的紫外扫描光谱图与目标化合物的特征吸收标准谱图比较，提高了定性分析的准确性。在优化的实验条件下，该方法显示出良好的线性关系（r〉0．999）和精密度（RSD〈10％），16种多环芳烃的检出限在0．005—1．33μg／kg之间，并成功应用于样品分析，样品加标回收率为71．4％～120％。实验中为了确保整个分析过程的可靠性，替代物的加标回收率控制在50％-150％之间；土壤标准参考物的测定结果都在预测值范围内，验证了该方法的准确性。

Determination of Polycyclic Aromatic Hydrocarbons in Soil by UPLC-DAD-FLD

A method using accelerated solvent extraction （ASE） and solid-phase clean-up to determine 16 polycyclic aromatic hydrocarbons （PAHs） in soils by ultra performance liquid chromatography） coupled with diode array detector and fluorescence detector （UPLC-DAD-FLD） was developed. Based on comparison of chromatographic column and optimization of detection wavelength, an analytical column with smaller particle size and inner diameter （ SupeleoSILTM LC-PAH, 100 × 3.0 i. d. ram, 3 μm） was selected. The method shortened analytical time, saved the solvent （acetonitrile） and met the requirement of fast and sensitive analysis for large quantity of samples through the improved detection wavelength. On the basis of qualitative analysis by retention times, a comparison of the ultraviolet spectrums of 16 PAHs obtained from PDA with their standard absorption spectrums were used to improve the accuracy. Under optimizing conditions, it showed good linearity （ r 〉 0. 999） and precision （ RSD 〈 10% ）. The detection limits for 16 PAH ranged from 0. 005 to 1.33 μg/kg. It had been applied to the analysis of samples successfully with spiked recoveries from soil samples in the range of 71.4% - -120%. In order to insure the reliability of the whole analysis, the spiked recoveries of substitutes were controlled in the range of 50% - 150%. The values obtained from standard soil reference object fell in the predicted range, which verified the accuracy of the method.