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建立了柱前衍生-高效液相色谱-荧光检测法(HPLC-FLD)测定皮革中全氟辛酸(PFOA)残留量的方法。以甲醇为萃取剂,室温下超声30min萃取皮革样品中的PFOA,以3-(溴乙酰基)香豆素(3-Br AC)为衍生剂,与PFOA发生衍生化反应,衍生产物通过HPLC-FLD测定,从而检测出PFOA的含量。结果表明:在浓度范围0.5~20mg/L内线性关系良好,最低检出限(LOD)为0.1mg/kg。在优化条件下,皮革样品中PFOA的加标回收率为89.0%~91.5%,相对标准偏差(RSD)为5.48%~6.92%。
A method of pre-column derivatization-high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of perfluorooctanoic acid (PFOA) residues in leather. PFOA was extracted from leather samples by sonication for 30 min at room temperature with methanol as extractant. Derivatization reaction of PFOA with PFOA by 3- (bromoacetyl) coumarin (3-Br AC) FLD assay to detect the level of PFOA. The results showed that there was a good linearity in the range of 0.5 ~ 20 mg / L with the lowest limit of detection (LOD) of 0.1 mg / kg. Under optimal conditions, the spiked recoveries of PFOA in leather samples ranged from 89.0% to 91.5% with relative standard deviations (RSDs) of 5.48% -6.92%.