经粉碎的橡胶样品用正己烷及丙酮(1+1)混合溶剂萃取,所得萃取液氮吹至近干后,加正己烷溶解残渣,将溶液经硅胶固相萃取柱净化,吸附于柱上的六溴环十二烷用正己烷-二氯甲烷(1+1)溶液淋洗,洗出液吹氮至近干,用乙腈溶解并用高效液相色谱法测定。选用Zorbax Eclipse XDB-C18色谱柱作固定相,用水-乙腈(15+85)溶液作流动相,紫外检测器测定波长为210 nm。方法的检出限(3S/N)为1.5 mg·kg-1。方法用于橡胶制品中六溴环十二烷的测定,回收率和测定值的相对标准偏差(n=7)分别在83.1%~94.3%和3.6%~6.4% 之间。

Samples of rubber products were crushed and extracted with mixed solvent of n-hexane and acetone (1+1). After evaporation of the extract to near dryness by N2-blowing, the residue was dissolved with n-hexane, and passed through the silica gel SPE column. Hexabromocyclododecane (HBCD) was adsorbed on the column and desorbed with an eluant containing n-hexane and CH2Cl2 (1+1). The eluate obtained was evaporated to near dryness by N2-blowing, and used for HPLC determination. Zorbax Eclipse XDB-C18 chromatographic column was used as stationary phase and mixed solution of H2O and acetonitrile (15+85) was used as mobile phase. UV-detection was made at 210 nm. Value of detection limit (3S/N) found was 1.5 mg·kg-1. The proposed method was applied to the determination of HBCD in rubber products, giving recovery and RSD′s (n=7) in the ranges of 83.1%-94.3% and 3.6%-6.4% respectively.