高效液相色谱法测定橡胶及其制品中16种多环芳烃  

HPLC Determination of 16 PAH′s in Rubber and Its Products

作　　者：王宏菊[1] 刘丽[1] 刘志红[1] 吴景武[1] 李英[1] 杨左军[1] 陈向阳[1] 陈麒宇[1] 李彬[1] 余淑媛[1] 

机构地区：[1]深圳出入境检验检疫局,深圳518045

出　　处：《理化检验（化学分册）》2009年第5期546-548,551,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局项目(2006B057)

摘　　要：经粉碎的橡胶样品用正己烷及丙酮（1＋1）的混合溶剂萃取，所得萃取液蒸至近干后加入正己烷2mL溶解残渣，将溶液经硅胶固相萃取柱分离并净化，吸附于柱上的多环芳烃用由正己烷及二氯甲烷（3＋2）组成的淋洗液解吸，洗出液蒸至近干加入一定量的内标溶液使之溶解并用高效液相色谱法测定。选用LC-PAH色谱柱作固定相，用乙腈和水以不同比例混合的溶液作为流动相进行梯度淋洗，紫外检测器的测定波长为210nm，以苝-d12作为内标进行定量测定，在优化的试验条件下16种多环芳烃可有效分离并测定。研究结果表明：16种多环芳烃的检出限（3S／N）、平均回收率及测定值的相对标准偏差（n=7）依次在0．05～0．10mg·L^-1，65．1％～101．7％及1．8％～7．3％之间。Rubber sample was crushed and extracted with mixed solvent of n-hexane and acetone （1 ＋ 1）. After evaporation of the extract to near dryness, the residue was taken up with 2 mL of rt-hexane, and passed through the silica gel SPE column. Polycyclic aromatic hydrocarbons （PAH＇s） were adsorbed on the column and desorbed with an eluant containing n-hexane and dichloromethane（3＋2）. The eluate obtained was evaporated to near dryness, dissolved with the internal standard solution, and used for HPLC determination. LC-PAH chromatographic column was used as stationary phase and mixed solutions of acetonitrile and water with different mixing ratio were used as mobile phase in the gradient elution. UV-detection were made at 210 nm. Under the optimized conditions, 16 PAH＇s in rubber were clearly separated, and determined with perylene-dlz as internal standard. Values of detection limit （3S/N）, average recovery and RSD＇s （n=7） obtained for the 16 PAH＇s were in the ranges of 0. 05-0. 10 mg · L^-1 , 65. 1%-101.7% and 1.8%-7. 3% respectively.

关 键 词：高效液相色谱法 多环芳烃 橡胶及其制品 

分 类 号：O652.63[理学—分析化学]