溶解沉淀-顶空气相色谱/质谱法测定丙烯酸树脂中残余单体

Determination of residual monomers in acrylic resin by dissolution precipitation-headspace-gas chromatography-mass spectrometry

建立了丙烯酸树脂中13种残余单体的溶解沉淀－顶空气相色谱／质谱检测方法。丙烯酸树脂样品用N，N-二甲基乙酰胺溶解后加去离子水沉淀，采用VF-624MS毛细管柱分离。13种残余单体能得到较好的分离，检出限（信噪比为3）为0．13～0．67mg／kg，定量限（信噪比为10）为0．33～2．01mg／kg，平均回收率为94．7％～113．4％，相对标准偏差（RSD）小于6％。

An analytical method for the quantitative determination of 13 residual monomers in acrylic resins by dissolution precipitation-headspace-gas chromatography-mass spectrometry has been developed. Acrylic resin was precipitated with water after dissolved with N, N-dimethylacetamide. The 13 acrylic monomers got a good separation on a VF-624 MS column. The limits of detection （LODs, S/N = 3 ） were between 0. 13 and 0.67 mg/kg, and the limits of quantification （ LOQs, S/N = 10） were in the range of 0.33 to 2.01 mg/kg for 13 analytes. Recoveries were in the range of 94.7% - 113.6%, with the relative standard deviations less than 6%. The method is simple, accurate and highly sensitive, and can be applied to analysis of the residual monomers in acrylic resins.