采用高效液相色谱-串联质谱法测定玩具弹性体中13种N-亚硝胺的含量。弹性体样品用模拟唾液浸泡,以Agilent Eclipse XDB-C18色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸水溶液和0.1%(体积分数)甲酸甲醇溶液的混合液为流动相进行梯度洗脱,采用电喷雾正离子源选择反应监测模式检测。13种N-亚硝胺的质量分数均在1~50 μg·kg-1范围内与其峰面积呈线性关系,方法的检出限(3s/k)在0.012~0.138 μg·kg-1之间。在1,5,50 μg·kg-1等3个浓度水平进行加标回收试验,回收率在77.4%~113%之间,测定值的相对标准偏差(n=6)在4.0%~12%之间。

HPLC-MS/MS was applied to the determination of 13 N-nitrosamines in elastomers of toys. The sample was extracted with simulated saliva. Agilent Eclipse XDB-C18 chromatographic column was used as stationary phase,and mixtures of 0.1% (φ) formic acid aqueous solution and 0.1% (φ) formic acid methanol solution mixed in various ratio were used as mobile phase in gradient elution. ESI+ and selected reaction monitoring mode were adopted in MS/MS. Linear relationships between values of peak area and mass fraction of 13 N-nitrosamines were kept in the same range of 1-50 μg·kg-1,with detection limits (3s/k) in the range of 0.012-0.138 μg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 1,5,50 μg·kg-1,giving values of recovery and RSD′s (n=6) in the ranges of 77.4%-113% and 4.0%-12%,respectively.