顶空气质联用法测定塑料制品中三聚甲醛和1,3-二氧戊烷残留量

Determination of 1,3,5-Trioxane and 1,3-Dioxolane Residues in Plastic Products by Headspace GC-MS

摘要: 建立了塑料制品中三聚甲醛和1,3-二氧戊烷残留量的顶空–气相色谱–质谱联用检测方法。样品以N,N-二甲基乙酰胺为溶剂溶解，经90℃，30 min静态顶空后，采用气质联用法测定，外标法定量。三聚甲醛和1,3-二氧戊烷在1.0~20 μg范围内呈良好线性关系，相关系数(r²)均大于0.999，方法定量限为1.0 mg/kg。1.0、2.0、5.0 μg添加水平下的加标回收率为91.8%~102%，RSD为2.8%~9.2% (n = 6)，该方法操作简便、准确可靠，可满足塑料制品中三聚甲醛和1,3-二氧戊烷残留量的定性和定量检测，可应用于塑料制品中三聚甲醛和1,3-二氧戊烷特定迁移量的筛检，节约成本，提高检测效率。

Abstract: A headspace gas chromatography-mass spectrometry (HS-GC-MS) method was developed for the determination of 1,3,5-trioxane and 1,3-dioxolane residues in plastic products. The sample was dissolved in N, N-Dimethylacetamide, and then determined by GC-MS after static headspace at 90˚C for 30 min. There was a good linear relationship between1,3,5-trioxane and 1,3-dioxolane in the range of 1.0~20 μg, the correlation coefficient (r²) was greater than 0.999, and the limit of quantita-tion was 1.0 mg/kg. The recoveries were 91.8%~102% with RSD of 2.8%~9.2% (n = 6) at the level of 1.0 μg, 2.0 μg and 5.0 μg. The method is simple, accurate and reliable. It can meet the requirements of qualitative and quantitative detection of the residues of 1,3,5-trioxane and 1,3-dioxolane in plastic products. It can be used to screen the specific migration of 1,3,5-trioxane and 1,3-dioxolane in plastic products, saving cost and improving detection efficiency.