LTQ-Orbitrap 组合式高分辨质谱测定纺织品中的15种邻苯二甲酸酯

摘要

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（3．5×100 mm ，3．5μm），以甲醇－5 mmol／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2．0 mg／kg ．按照建立的方法进行了2．0、5．0和10．0 mg／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．%The analysis of 15 phthalates esters was evaluated using high performance liquid chromatography(HPLC)combined with full-scan accurate linear ion trap-orbitrap mass spec-trometry(LTQ-Orbitrap) .The textiles were extracted with methanol .The LC separation was performed on a column of Agilent Eclipse XDB-C18 (3 .5 × 100 mm ,3 .5 μm)with methanol and 5 mmol/L ammonium acetate (0 .1% formic acid ,V /V ) solution as the mobile phase .The phthalates esters were detected by FT positive mode .The external standard calibration showed good linearity within the concentrations of 0 .05 - 5 .0 mg/L for all phthalates esters .The corre-lation coefficient is more than 0 .99 ,and the limit of detection is 2 .0 mg/kg .The average recov-eries of 15 phthalates esters ranged from 81 .3% to 103 .2% at the spiked levels of 2 .0 ,5 .0 and 10 .0 mg/kg with the relative standard deviations (RSDs) less than 12 .9% .We have developed the method based on accurate mass measurements of extracted target ions in full scan mode u-sing LC-LTQ-Orbitrap XL and ToxID as a tool for fast quantitative analysis .The instrument exhibited very high sensitivity and repeatability .