基于氮化碳复合材料磁性固相萃取结合高效液相色谱法测定尿液中3种羟基多环芳烃

建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料,经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后,用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积(单次洗脱体积×洗脱次数)对萃取效率的影响。结合高效液相色谱-荧光分析,在0.25～250μg/L范围内线性关系良好(相关系数r=0.999), 3种羟基多环芳烃的检出限和定量限分别为0.08和0.25μg/L,回收率为90.1%～102%,日内和日间精密度分别为1.5%～7.7%和2.2%～8.7%。该本方法简单、快速、高效,可用于尿液中羟基多环芳烃的分析。

Determination of three hydroxyl polycyclic aromatic hydrocarbons in urine using magnetic solid-phase extraction with magnetic carbon nitride composites coupled with high performance liquid chromatography

A method based on the magnetic solid-phase extraction using magnetic carbon nitride composites coupled with high performance liquid chromatography-fluorescence detector (HPLC-FLD) was developed for the simultaneous determination of three hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine. The synthesized sorbent was characterized by scanning electron microscope, X-ray diffractometer, vibrating sample magnetometer and surface area analyzer. The extraction parameters such as amount of sorbent, extraction time, eluting solvent and volume (single eluting volume×eluting times) were investigated in detail. Under the optimized conditions, the method showed a linear range of 0.25-250 μg/L (correlation coefficient=0.999). The limit of detection was 0.08 μg/L and the limit of quantification was 0.25 μg/L for each analyte. The proposed method gave a recovery of 90.1%-102%. The relative standard deviations for the intra-day and inter-day were 1.5%-7.7% and 2.2%-8.7%, respectively. The feasibility of the developed method was further demonstrated during the analysis of real samples. The results indicate that the magnetic carbon nitride composites can be used for the effective purification and enrichment of three OH-PAHs in urine. In addition, the method can be applied for analysis of urinary OH-PAHs in a simple, fast, and effective manner.