超高效液相色谱-质谱法测定环氧树脂粘结剂中双酚A  

UHPLC-MS Determination of Bispheol A in Epoxy Resin Adhesives

作　　者：赖莺[1] 董清木[1] 林睿[1] 葛秀秀[1] 蔡延平[1] 林海霞[1] 

机构地区：[1]厦门出入境检验检疫局技术中心,厦门361026

出　　处：《理化检验（化学分册）》2013年第4期448-450,454,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局课题(2011IK048;2009IK075)

摘　　要：提出了环氧树脂粘结剂中双酚A的超高效液相色谱-质谱测定方法。样品用乙醇超声提取后,离心分离,取上清液过0.22μm有机滤膜,滤液经ZORBAX SB-C18色谱柱分离,用不同比例的水和乙腈的混合溶液作为流动相梯度淋洗,采用电喷雾负离子源,多反应监测模式。双酚A的质量浓度在2～1 000μg.L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为0.5mg.kg-1。以空白环氧树脂粘结剂为基体,进行加标回收试验,测得回收率在89.3%～93.2%之间,测定值的相对标准偏差(n=6)在1.8%～3.3%之间。UHPLOMS was applied to the determination of bisphenol A in epoxy resin adhesives. Sample of epoxy resin adhesives was extracted by ethanol, after centrifugation, the clear super natant obtained was filtrated with 0. 22μm organic filtration membrane. The filtrate was used for UHPLC-MS determination, in which ZORBAX SB-C18 column was used as chromatographic column, and mixtures of water and acetonitrile of different proportions were used as mobile phase in gradient elution; negative electrospray ionization as well as multiple reaction monitoring mode was used in the detection. Linear relationship between value of peak area and mass concentration of bisphenol A was obtained in the range of 2--1 000 μg·L^-1 , with quantification limit （lOS^N） of 0. 5 mg·kg^-1. Tests for recovery and precision were made by addition of standard solution of bispheol A to blank sample of epoxy resin adhesives which was then analyzed by the proposed method. Values of recovery and RSD＇s （n = 6） obtained were in the ranges of 89.3%--93.2% and 1.8%--3.3% respectively.

关 键 词：超高效液相色谱-质谱法 双酚A 环氧树脂 粘结剂 

分 类 号：O657.63[理学—分析化学]