毛细管SPE-GC法测定纺织品中邻苯二甲酸酯

Determination of phthalate esters in textiles by in-tube capillary SPE-GC method

建立了新型毛细管固相萃取-气相色谱法检测纺织品中邻苯二甲酸酯（PAEs）的方法。通过比较筛选出毛细管固相萃取柱的最佳萃取剂，并优化萃取条件，净化富集待测物质后与气相色谱联用进行定性定量检测。采用的毛细管内固相萃取条件为：选取C18中的萃取剂为毛细管固相萃取剂，1．2μL甲醇和1．2μL超纯水依次活化，上样速率0．5μL／min，热脱附。该方法在1-1000μg／L质量浓度范围内线性关系良好；DMP、DEP和DBP的最低检出限分别是4．1μg／L、4．8μg／L和5．4μg／L；加标回收率分别是84％-99％、88％-97％和84％-98％；相对标准偏差（RSD）分别为5．34％、4．23％和6．02％。

An in-tube capillary solid-phase extraction （SPE）-gas chromatography （GC） method is devel- oped for determination of dimethyl phthalate（DMP）, diethyl phthalate（DEP） and dibutyl phthalate（DBP） in textiles. The optimal extraction conditions are using extractant in C18 as solid phase extractant, using 1.2 μL methanol and 1.2μL ultrapure water to activate the extraction column, sampling rate 0.5 μL/min, thermal desorption. The method shows good linear relationship in the range of 1-1 000μg/L. The detec- tion limits of DMP, DEP and DBP are 4.1 μg/L, 4.8 μg/L and 5.4 μg/L. The recoveries are 84%-99%, 97%- 98% and 84%-88% respectively. The relative standard deviation are 5.34%,4.23% and 6.02%.