气相色谱-质谱法测定涂料中的六溴环十二烷

GC-MS Determination of Hexabromocyclododecane in Coatings

提出了用气相色谱-质谱法测定涂料中六溴环十二烷含量的方法。样品用二氯甲烷-丙酮(1+1)混合溶剂超声提取,提取液经硅胶固相萃取小柱净化、平行蒸发定量浓缩后,用DB-5MS毛细管柱进行分离,全扫描模式和选择离子监测模式测定。六溴环十二烷的质量浓度在1～50mg·L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为10 mg·kg-1。添加5,20,50mg·L-1 3个浓度水平进行加标回收试验,回收率在82.0%～106%之间,测定值的相对标准偏差(n=8)在2.8%～5.3%之间。

A method for the determination of hexabromocyclododecane （HBCD） in coatings by GC-MS was proposed. Sample was ultrasonically extracted with dichloromethane-acetone （1＋1） mixed solvent, purified by passing through silica gel solid phase extraction column, and quantitatively concentrated with parallel evaporation instrument. DB-SMS capillary column was used for separation, and full-scanning mode and selected ion monitoring mode were adopted in MS determination. Linear relationship between values of peak area and mass concentration of HBCD was kept in the range of 1-50 mg . L^-1, with lower limit of determination （10S/N） of 10 mg . kg^-1. Tests for recovery were made at the concentration levels of 5, 20, 50 mg . L^-1 of HBCD standard, giving values of recovery and RSD＇s （n=8） in the ranges of 82. 0%--106% and 2.8%-5.3% respectively.