超声萃取/气相色谱-串联质谱法同时测定皮革制品中20种邻苯二甲酸酯类增塑剂

Simultaneous Determination of 20 Kinds of Phthalate Plasticizers in Leather Products by Gas Chromatography-Tandem Mass Spectroscopy Coupled with Ultrasonic Extraction

建立了同时测定皮革制品中20种邻苯二甲酸酯类增塑剂的气相色谱-串联质谱方法。该方法以正己烷为提取溶剂,室温下超声提取皮革制品中的邻苯二甲酸酯类增塑剂,提取液经中性氧化铝固相萃取柱净化后进行气相色谱-串联质谱分析。该方法简便快速,定性定量准确,灵敏度高,DIDP、DINP和DMPP的定量下限(S/N=10)分别为0.2、0.2、0.1 mg/kg,其余17种邻苯二甲酸酯类增塑剂的定量下限均小于50μg/kg,RSD小于12%,平均加标回收率为86%～95%。采用该方法对47个市售皮革制品进行测定,结果在2个样品中检出多种邻苯二甲酸酯类增塑剂。

An effective GC-MS/MS method was established for the simultaneous determination of contents of 20 phthalate plasticizers in leather products.The phthalate plasticizers in leather products were ultrasonically extracted at room temperature using hexane as the extraction solvent,then the extract was purified with neutral alumina solid extraction column,followed by analysis of gas chromatography-tandem mass spectrometry.The method was simple,rapid,sensitive and accurate.The limits of quantitation（LOQ,S/N=10） of DIDP,DINP and DMPP were 0.2,0.2 and 0.1 mg/kg,respectively,while the LOQs for the other 17 phthalate plasticizers were all less than 50 μg/kg.The relative standard deviations（RSDs） of the method were all less than 12% ,and the spiked average recoveries ranged from 86% to 95%.The proposed method was applied in the determination of phthalate plasticizers in 47 commercially available leather products,and two of which were detected containing phthalate plasticizers.