采用超高效液相色谱-串联质谱法测定食品包装材料中18种邻苯二甲酸酯的含量。食品包装材料样品用正己烷提取,采用Aglient ZDRBAX RRHD Eclipse Plus C18色谱柱(3.0 mm×100 mm,1.8 μm),同时串联ZORBAX Eclipse Plus C18富集柱(2.1 mm×50 mm,1.8 μm),以不同体积比的0.1%(体积分数)甲酸水溶液和甲醇的混合液作为流动相梯度洗脱,采用电喷雾正离子源多反应监测模式检测。18种邻苯二甲酸酯的质量浓度均在0.050~5.0 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.003~0.030 mg·kg-1之间。在0.1,1.0,10.0 mg·kg-1等3个浓度水平进行加标回收试验,回收率在87.5%~102%之间,测定值的相对标准偏差(n=6)在0.90%~3.9%之间。

UPLC-MS/MS was applied to the determination of 18 phthalate esters in food packing materials. Sample of food packing material was extracted with n-hexane. Separation was performed on Aglilent ZDRBAX RRHD Eclipse Plus C18 column (3.0 mm×100 mm, 1.8 μm) connected in series with ZORBAX Eclipse Plus C18 column (2.1 mm×50 mm, 1.8 μm). Mixtures of 0.1% (φ) fomic acid solution and methanol mixed in different ratio were used as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 18 phthalates were kept in the same range of 0.050-5.0 mg·L-1, with detection limits (3S/N) in the range of 0.003-0.030 mg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 0.1,1.0,10.0 mg·kg-1, giving values of recovery and RSD′s (n=6) in the ranges of 87.5%-102% and 0.90%-3.9% respectively.