气相色谱-质谱联用法检测水性墙体涂料中20种邻苯二甲酸酯

Determination of Twenty Phthalic Acid Esters in Waterborne Wall Coatings by Gas Chromatography-Mass Spectrometry

建立了一种检测水性墙体涂料中20种邻苯二甲酸酯的分散固相萃取净化（d-SPE）/气相色谱-质谱联用（GC-MS）分析方法.样品经水分散,乙腈-叔丁基甲醚（9∶1）提取后,以无水硫酸镁（MgSO4）和N-丙基乙二胺（PSA）粉末分散固相萃取净化,GC-MS法测定,外标法定量.20种邻苯二甲酸酯在0.01～10 mg/L范围内线性关系良好（r＞0.99）,方法的检出限（LOD）为0.07～ 1.40 mg/kg,定量下限（LOQ）为0.3～4.7mg/kg,加标回收率为86.3％～115.3％,相对标准偏差（RSD,n=6）小于8％.该方法净化效果好、定量准确,适用于水性墙体涂料中20种邻苯二甲酸酯的快速检测.

A method was established for the determination of 20 phthalic acid esters （PAEs） in water- borne wall coatings by gas chromatography -mass spectrometry（ GC -MS） after dispersive solid phase extraction（d-SPE） cleanup. The samples were dispersed with water, and stirred uniformly, then ex- tracted with acetonitrile- methyl tert-butyl ether（9 ： 1 ）. The ultimate solution was detected by GC - MS under selected ion monitoring mode and quantified by the external standard method. The calibra- tion curves of 20 PALEs were linear in the range of 0. 0i -10 mg/L with correlation coefficients （r） more than 0.99. The limits of detection （LODs） of the method for target compounds ranged from 0. 07 mg/kg to 1.40 mg/kg, and the limits of quantitation of the method （LOQs） varied from 0. 3 mg/kg to 4. 7 mg/kg. The mean recoveries ranged from 86. 3% to 115.3% with relative standard de- viations （RSDs） less than 8%. This method was suitable for the identification and quantification of 20 PAEs in waterborne wall coatings due to its simplicity and accuracy.