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建立了线性离子阱-静电场轨道肼高分辨质谱(LTQ-Orbitrap)快速同时测定纺织品中15种邻苯二甲酸酯残留的方法,并根据精确地分子离子峰和子离子峰进行定性和确证.样品经甲醇提取,用Agilent Eclipse XDB-C18色谱柱(3.5×100mm,3.5μm),以甲醇-5mmol/L乙酸铵(含0.1%甲酸,V/V)溶液为流动相,FT正离子扫描模式进行质谱检测,外标法定量.结果表明,该方法在0.05~5.0 mg/L范围内线性关系良好(r≥0.99),检出限为2.0mg/kg.按照建立的方法进行了2.0、5.0和10.0mg/kg 3个添加水平的15种邻苯二甲酸酯的加标回收试验,回收率为81.3%~103.2%,相对标准偏差为5.7%~12.9%.本文利用LTQ-Orbitrap高分辨质谱配合全自动筛选应用软件ToxID可以对大量数据文件进行高通量分析的特点,建立了纺织品中15种邻苯二甲酸酯残留的快速筛选和确证方法.
A method for rapid and simultaneous determination of 15 phthalate residues in textiles by linear ion trap-electrostatic field orbit hydrazine high-resolution mass spectrometry (LTQ-Orbitrap) was established and characterized according to the accurate molecular ion and ion peaks. The samples were extracted with methanol and analyzed by Agilent Eclipse XDB-C18 column (3.5 × 100mm, 3.5μm) with methanol-5mmol / L ammonium acetate solution containing 0.1% formic acid and V / V as mobile phase. The results showed that the method has a good linearity (r≥0.99) in the range of 0.05-5.0 mg / L with a detection limit of 2.0 mg / kg.According to the established method, 2.0, 5.0 And 10.0mg / kg three added levels of 15 kinds of phthalates spiked recovery test, the recovery rate was 81.3% ~ 103.2%, the relative standard deviation of 5.7% ~ 12.9% .This paper uses LTQ-Orbitrap high resolution Mass spectrometry combined with ToxID, a fully automated screening application, enables high-throughput analysis of a large number of data files and establishes a rapid screening and confirmation method for 15 phthalate residues in textiles.