Xu Bingbing, Li Xiaomin, Zhang Qinghe, Zhu Weihuang
School of Environmental and Municipal Engineering, Xi'an University of Architecture & Technology, Xi'an 710055, China.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China.
Se Pu. 2018 Aug 8;36(8):786-794. doi: 10.3724/SP.J.1123.2018.03010.
A method was established for the determination of 16 phthalate acid esters (PAEs) in infant formula by gas chromatography-tandem mass spectrometry (GC-MS/MS). PAEs in infant formula samples were homogenized by deionized water, extracted with acetonitrile, and purified by a solid-phase extraction (SPE) method using primary secondary amine (PSA) sorbents. The separation was performed on a DB-5 MS UI (30 m×0.25 mm×0.25 μm) capillary column. Effects of different elution solvents on alumina/PSA and PSA SPE columns were investigated. Fair recoveries of 16 PAEs were achieved on the PSA column upon elution by mixed -hexane-acetone (60:40, v/v). All the 16 PAEs were quantified by matrix-matched isotopic-dilution mass spectrometry (IDMS); the 16 PAEs showed linear relationships in the concentration range of 0.01-2.0 mg/kg with linear coefficients () greater than 0.9996. The limits of detection (LODs) and quantification (LOQs) were in the range of 0.15-2.5 μg/kg and 0.50-8.33 μg/kg, respectively. The recoveries of the 16 PAEs, obtained using the IDMS method, were 96.1%-104.0% with relative standard deviations (RSDs) lower than 3.3% (=5). These results established the method described here as sensitive and precise for the simultaneous determination of 16 PAEs in infant formula, even at trace concentrations.
建立了一种采用气相色谱 - 串联质谱法（GC-MS/MS）测定婴幼儿配方奶粉中16种邻苯二甲酸酯（PAEs）的方法。婴幼儿配方奶粉样品中的PAEs用去离子水匀浆，乙腈萃取，并用伯仲胺（PSA）吸附剂通过固相萃取（SPE）方法进行净化。在DB-5 MS UI（30 m×0.25 mm×0.25 μm）毛细管柱上进行分离。研究了不同洗脱溶剂对氧化铝/PSA和PSA SPE柱的影响。在PSA柱上用正己烷 - 丙酮混合液（60:40，v/v）洗脱时，16种PAEs均获得了良好的回收率。所有16种PAEs均采用基质匹配同位素稀释质谱法（IDMS）进行定量；16种PAEs在0.01 - 2.0 mg/kg浓度范围内呈线性关系，线性系数（）大于0.9996。检测限（LODs）和定量限（LOQs）分别在0.15 - 2.5 μg/kg和0.50 - 8.33 μg/kg范围内。采用IDMS方法获得的16种PAEs的回收率为96.1% - 104.0%，相对标准偏差（RSDs）低于3.3%（=5）。这些结果表明，本文所述方法对于同时测定婴幼儿配方奶粉中痕量浓度的16种PAEs具有灵敏性和精确性。
