高效液相色谱-质谱法测定压敏胶及其制品中9种邻苯二甲酸酯

Determination of Nine Phthalate Esters in Pressure-sensitive Adhesive and Its Products by High Performance Liquid Chromatography-Mass Spectrometry

采用高效液相色谱-质谱（HPLC-MS）法,对压敏胶及其制品中的9种邻苯二甲酸酯进行同时测定。以乙酸乙酯为溶剂溶解压敏胶,甲醇沉淀高聚物,以3 000 r/min离心5 min,清液定容后,用HPLC-MS分析检测。采用Xterra-Phenyl色谱柱,流动相为乙腈-水,流速为1 mL/min,选择离子监测。在优化实验条件下,9种邻苯二甲酸酯在0.1~10 mg/L范围内线性关系良好;DIBP、BBP、DEHP、DNOP的方法定量下限（LOQ）为0.000 1%,DMP、DEP、DBP、DINP、DIDP为0.000 5%。对常用的热熔型压敏胶、溶剂型压敏胶和乳液型压敏胶的空白基体进行加标回收实验,加标回收率为88%~110%,相对标准偏差（RSD）不大于6.1%。该方法简单、快速、灵敏,能满足压敏胶及其制品中邻苯二甲酸酯的分析要求。

A high performance liquid chromatography-mass spectrometric（HPLC-MS） method was developed for the simultaneous determination of nine phthalate esters（PAEs） in pressure-sensitive adhesive and its products.The sample was dissolved with ethyl acetate,and the PAEs were separated from polymer by using methanol.The extract was centrifugally separated for 5 min at a speed of 3 000 r/min,and the nine PAEs were separated on an Xterra-Phenyl（150 mm×3.9 mm,5 μm） column by gradient elution using acetonitrile-water as the mobile phase at a flow rate of 1 mL/min,and quantitatively determined under selected ion monitoring（SIM）.Under the optimized conditions,the method showed a good linearity in the range of 0.1-10 mg/L for the nine PAEs.The limits of quantitation were 0.000 1% for DIBP,BBP,DEHP and DNOP,and 0.000 5% for DMP,DEP,DBP,DINP and DIDP.The established method was applied in the determination of three kinds of common pressure-sensitive adhesives,e.g.hotmelt pressure-sensitive adhesive,solvent pressure sensitive adhesive and emulsion pressure-sensitive adhesive.The results indicated that the recoveries ranged from 88% to 110% with relative standard deviations（RSDs） less than 6.1%.The method was reliable,sensitive and reproducible,and could meet the requirements of determination of PAEs in pressure-sensitive adhesive and its products.