顶空气相色谱-质谱联用法测定胶粘剂中的残余单体

建立了一种测定胶黏剂中6种丙烯酸酯和甲基丙烯酸酯类残余单体的分析方法。样品经100 ℃、30 min顶空加热后,通过DB-WAX色谱柱(30 m×0.25 mm×0.25 μm)分离和质谱选择离子模式检测,内标法定量。结果表明,6种残余单体能达到良好的分离,检出限(信噪比为3)为0.069～0.096 mg/kg,定量限(信噪比为10)为0.23～0.32 mg/kg,平均回收率为96.0%～104.6%,相对标准偏差(RSD)小于7.2%。该方法操作简便、准确、重复性好、灵敏度高,可用于胶黏剂中丙烯酸酯和甲基丙烯酸酯类残余单体的快速测定。

Determination of residual acrylate monomers in adhesives by headspace gas chromatography-mass spectrometry

A method was developed for the determination of methyl acrylate, ethyl acrylate, butyl acrylate, methyl methacrylate, ethyl methacrylate and butyl methacrylate in adhesives by headspace gas chromatography-mass spectrometry (HS-GC-MS). The samples were treated at 100 degrees C for 30 min, then separated on a DB-WAX column (30 m x 0.25 mm x 0.25 microm) and determined by MS under selected ion monitoring mode and quantified by internal standard method. The established method showed good separation with the limits of detection (LODs, S/N = 3) of 0.069 - 0.096 mg/kg and the limits of quantification (LOQs, S/N = 10) of 0.23 - 0.32 mg/kg. The recoveries for acrylate monomers were in the range from 96.0% to 104.6% with the relative standard deviations less than 7.2%. The method is simple, accurate, rapid and highly sensitive. It can be applied to analyze the residual acrylates and methyl acrylates in adhesives.