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  

HPLC-MS/MS Determination of 13 N-Nitrosamines in Elastomeric Material of Toys

作　　者：费桂琴[1] 陈山丹[1] 白桦[2] 李敬[1] 

机构地区：[1]江苏出入境检验检疫局轻工产品与儿童用品检测中心,扬州225009 [2]中国检验检疫科学研究院,北京100123

出　　处：《理化检验（化学分册）》2015年第11期1529-1533,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技计划项目(2011IK114)

摘　　要：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1~50μg·kg-1范围内与其峰面积呈线性关系,方法的检出限（3s/k）在0.012~0.138μg·kg-1之间。在1,5,50μg·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 Nnitrosamines were kept in the same range of 1-50μg·kg-1,with detection limits（3s/k）in the range of 0.012-0.138μg·kg-1.Tests for recovery were made by standard addition method at the concentration levels of 1,5,50μg·kg-1,giving values of recovery and RSD′s（n=6）in the ranges of 77.4%-113% and 4.0%-12%,respectively.

关 键 词：高效液相色谱-串联质谱法 玩具 弹性体 N-亚硝胺 

分 类 号：O657.63[理学—分析化学]