微波辅助萃取-气相色谱-串联质谱法同时测定皮革制品中20种邻苯二甲酸酯含量

Simultaneous Determination of 20 Phthalates in Leather Products by Microwave-Assisted Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

为了加强对皮革制品中邻苯二甲酸酯的监管,建立了气相色谱-串联质谱法同时测定皮革制品中的20种邻苯二甲酸酯。该方法以乙腈为萃取溶剂,微波萃取皮革制品中的邻苯二甲酸酯,萃取液经固相萃取柱净化后,气相色谱-串联质谱分析。在S/N=10条件下,邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)和邻苯二甲酸二(4-甲基-2-戊基)酯(DMPP)的定量下限分别为0.2、0.2、0.1mg/kg,其余邻苯二甲酸酯的定量下限均小于0.05mg/kg,平均加标回收率为87.75%～94.59%,精密度实验RSD均小于16%。采用该方法对市售皮革制品进行测定,在2个样品中检出多种邻苯二甲酸酯。

In order to strengthen the supervision of phthalates in leather products, a method for the simultaneous determination of 20 phthalates in leather products was established. Phthalates in leather products were extracted by microwave-assisted extraction （MAE） using acetonitrile as solvent, the extracts were purified by solid-phase extraction, and then analyzed using gas chromatography-tandem mass spectrometry （GC-MS/MS）. At the condition of S/N=10, the limits of quantification are 0.2, 0.2 and 0.1 mg/kg for DINP, DIDP and DMPP, respectively, while the limits of quantification are all less than 0.05 mg/kg for other phthalates. The spiked average recoveries vary from 87.75% to 94. 59%. The relative standard deviation （RSD） of precision experiment is less than 16%. The proposed method was applied to the analysis of commercially available leather products, and phthalates were found to exist in two samples.