磁固相萃取-液相色谱法测定环境水样中有机紫外防晒剂

Determination of organic ultraviolet filters in environmental waters by magnetic solid phase extraction-high performance liquid chromatography

采用自制的聚离子液体功能化磁性材料有效富集有机紫外防晒剂,并与高效液相色谱-二极管阵列检测器(HPLC-DAD)联用,建立了环境水样中痕量有机紫外防晒剂的检测方法。研究系统考察了解吸溶剂、吸附和解吸时间、样品pH值、离子强度等因素对萃取性能的影响。在最佳萃取条件下,水杨酸辛酯的线性范围为0 5~200 0μg/L,其他有机紫外防晒剂的线性范围为0 2~200 0μg/L;6种目标物的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0 009~0 13μg/L和0 031~0 43μg/L。所建方法成功用于实际环境水样中有机紫外防晒剂的测定,不同加标水平下目标物的加标回收率为71 4%~120%,相对标准偏差均低于10%。研究表明,所建方法具有操作简便、萃取速度快、灵敏度高和环境友好等特点,可用于环境水样中有机紫外防晒剂的检测。

A method for the determination of organic ultravioletfilters (OUFs) in water samples was developed by the combination of polymeric ionic liquid-based magnetic solid-phase extraction (PIL-MSPE) and high performance liquid chromatography-diode array detection (HPLC-DAD).To achieve the optimum extraction performance for the target analytes,several key variables,including desorption solvent,adsorption and desorption time,sample pH value and ionic strength in the sample matrix,were investigated in detail.Under the most favorable extraction conditions,linear behaviors were observed in the ranges of 0.5-200.0 μg/L for octyl salicylate and 0.2-200.0 μg/L for the other analytes.The limits of detection (LODs,S/N=3) and limits of quantification (LOQs,S/N=10) for the target OUFs were in the ranges of 0.009-0.13 μg/L and 0.031-0.43 μg/L,respectively.The developed PIL/MSPE-HPLC-DAD method was successfully applied to detect trace OUFs in real water samples.The spiked recoveries at different spiked levels were 71.4%-120%,and the RSDs were below 10% for all the compounds in all the samples.The proposed method has some unique merits including simple operation,fast extraction procedure,high sensitivity and environmental friendliness.It can become a useful method for the monitoring of trace OUFs in water samples.