气相色谱-串联质谱法测定生态纺织品中的邻苯二甲酸酯类

Determination of Phthalate Esters in Ecological Textile by GC-MS/MS

采用气相色谱-串联质谱法同时测定生态纺织品中的24种邻苯二甲酸酯类。样品经正己烷超声提取,提取液经ProElut PSX玻璃固相萃取柱净化,以丙酮-正己烷(15+85)混合液洗脱,洗脱液经氮气吹至近干后,用正己烷定容至1.0 mL。采用DB-5MS毛细管色谱柱分离,质谱分析中采用电子轰击离子源和选择反应监测模式。24种邻苯二甲酸酯类的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在1.0~10 mg·kg^(-1)之间,测定下限(10S/N)在5.0~25 mg·kg^(-1)之间。加标回收率在81.3%~102%之间,测定值的相对标准偏差(n=6)在1.8%~6.6%之间。

GC-MS/MS was applied to the determination of 24 phthalate esters in ecological textiles. The sample was extracted with hexane. Then the extract was cleaned up by using ProElut PSX glass SPE column, with a mixture of acetone and hexane as eluant. The eluant was concentrated to dryness by N2 blowing and diluted to 1.0 mL with hexane. The anaiytes were separated on a DB-5MS capillary chromatographic column. EI and SRM were adopted in MS analysis. Linear relationships were found between the peak areas and the mass concentrations of 24 phthalate esters in definite ranges, with detection limits （3S/N） in the range of 1.0-10 mg·kg^-1 and the lower limits of determination （10S/N） in the range of 5.0-25 mg·kg^-1. Recovery rates obtained by standard addition method were in the range of 81.3%-102%, and RSDs （n=6） were in the range of 1.8%-6.6%.