分散固相萃取净化气相色谱-质谱联用法快速检测纸质包装材料中18种光引发剂

Simultaneous Determination of 18 Photoinitiators Residues in Paper-made Packaging by Gas Chromatograph-Mass Spectrometry after Dispersive Solid Phase Extraction Cleanup

建立了一种分散固相萃取(d-SPE)净化、气相色谱-质谱联用法(GC-MS)检测纸质包装材料中18种光引发剂(PIs)的分析方法。样品经水浸润后,用乙腈对样品进行超声提取,提取液经正己烷-乙酸乙酯溶液(3∶7,V/V)液液萃取后,用无水MgSO4、N-丙基乙二胺(PSA)和C18粉末分散固相萃取净化,以GC-MS法测定,内标法定量。18种PIs在0.01～0.2 mg/L内线性关系良好(R2>0.997),3个加标水平(0.1,0.4和2 mg/m2)的回收率在81.6%～123.8%之间,相对标准偏差(RSD)为0.2%～9.6%,检出限(LOD)为0.007～0.023 mg/m2。结果表明:本方法简便、测定结果准确,可用于纸质包装材料中18种光引发剂残留的高通量检测。

A method was developed for the simultaneous determination of 18 photoinitiators（PIs） residues in paper-made packaging by gas chromatograph-mass spectrometry（GC-MS） after dispersive solid phase extraction（d-SPE） cleanup.PIs were ultrasonically extracted by acetonitrile from water presoaked sample,followed by liquid-liquid distribution extraction with n-hexane-acetic ether（3 ∶ 7,V/V） and cleaned up by the mixed sorbents of anhydrous MgSO4 plus primary secondary amine（PSA） and octadecylsilane（C18） sorbent power.The ultimate solution was detected and quantified by GC-MS under selected ion monitoring mode by using anthracene D10 as the internal standard.All of the 18 PIs had good linear relationship（R2 0.997） in the concentrations of 0.01 to 0.2 mg/L.The recoveries of 18 PIs were in the range from 81.6% to 123.8% at three spike levels of 0.1,0.4 and 2 mg/m2 with relative standard deviation（RSD） less than 9.6%.The detection limits of target compounds in the method were ranged from 0.007 mg/m2 to 0.023 mg/m2.The real sample analysis showed that this simple and accurate method could be used for the determination of the residues of 18 PIs simultaneously in the paper-made packaging sample.