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

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5min,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...

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

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.