新型毛细管内固相萃取-气相色谱法检测纺织品中烷基酚类物质

摘要

建立了毛细管内固相萃取（ SPE）-气相色谱（ GC）检测纺织品中壬基酚和辛基酚含量的分析方法。通过比较4种性质不同固相萃取剂的萃取效果，筛选出对烷基酚（ APs）类物质萃取效果最佳的固相萃取剂，将其作为填充物质制作毛细管内固相萃取柱，将毛细管内固相萃取法与气相色谱联用进行分析检测。最佳固相萃取剂为 Abselut NEXUS，毛细管内固相萃取最佳条件为：1.2μL 甲醇和1.2μL 超纯水活化，1.2μL 甲醇洗脱，上样速率是0.4μL／min。该法在较低浓度范围内呈现良好的线性相关性，对烷基酚的富集倍数约为100倍，对辛基酚和壬基酚的检出限分别为3.7μg／L和4.5μg／L，加标回收率分别为85.6％~98.2％和83.8％~95.7％，结果表明，此法能够简捷、迅速、有效地检测出纺织品中残留的烷基酚类物质。%An in-tube capillary solid-phase extraction( SPE)-gas chromatography( GC)meth-od was developed for confirmation and quantitative determination of octylphenol ( OP ) and nonylphenol( NP)in textiles. To make the in-tube capillary SPE column,the best SPE car-tridge was chosen from four kinds of SPE cartridges. The adsorbent in the cartridge was used as the filling material to make the in-tube capillary SPE column. The nature,volume used,flow rate and adsorption capacity of the eluent were compared. Finally,the in-tube capillary solid-phase extraction was combined with gas chromatography to detect the alkyl phenols( APs ). Abselut NEXUS extraction cartridge was chosen as the best solid phase extractant. The optimal in-tube capillary SPE extraction conditions were as follows:1. 2 μL methanol and 1. 2 μL ultra-pure water for activating the extraction column,1. 2 μL methanol for eluting,0. 4 μL/min for solution loading. The method showed a good linear relationship in the low concentration range, and the enrichment ratios for the APs were about 100 times. The detection limits of octylphenol and nonylphenol were 3. 7 μg/L and 4. 5 μg/L,respectively. The recoveries of octylphenol were 85. 6%-98. 2%,and those of nonylphenol were 83. 8%-95. 7%. The experimental results demon-strated that the method is simple,rapid,and useful for detecting APs in textiles.