提出了气相色谱-质谱法检测奶嘴中3种磷酸苯酚酯［磷酸三甲苯酯(TCP)、磷酸甲苯二苯酯(CDP)和磷酸三-二甲苯酯(TXP)］的方法。试样经乙酸乙酯提取后,在35 ℃水浴中在40 ℃旋转蒸发仪中浓缩后,用甲醇溶解定容至2.0 mL,通过DB-1701石英毛细管色谱柱(30 m×0.25 mm,0.15 μm)分离,采用电子轰击离子源选择离子检测模式进行质谱测定。3种磷酸苯酚酯质量浓度均在30.0~500 μg·L-1内与其峰面积呈线性关系,测定下限(10S/N)为30 μg·kg-1。以奶嘴样品为基体加入3种浓度水平的混合标准溶液按方法测定后,求得方法的回收率在64.0%~88.5%之间,相对标准偏差(n=10)为0.86%~8.7%。

A method for determination of 3 phenol phosphates i.e., tricresyl phosphate (TCP), cresyl diphenyl phosphate (CDP) and trixylenyl phosphate (TXP), in nipple by GC-MS was proposed. The 3 phenol phosphates in sample was extracted with ethyl acetate, and the extracts were concentrated by rotary evaporator in a water bath at 35 ℃. The residue obtained was dissolved and made up to 2.0 mL with methanol, which was used for GC-MS analysis. The DB-1701 capillary chromatographic column (30 m×0.25 mm, 0.15 μm) was used for separation, and the electron impact ionization source with selected ion monitoring (SIM) was adopted in MS. Linear relationships were obtained between values of peak area and mass concentration of the 3 phenol phosphates in the same range of 30.0-500 μg·L-1, with lower limit of determination (10S/N) of 30 μg·kg-1. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery and RSD′s (n=10) found were in the ranges from 64.0% to 88.5% and 0.86% to 8.7% respectively.