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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.

参考文献

[1] Sung HH;Ye YZ.Effect of nonylphenol on giant freshwater prawn (Macrobrachium rosenbergii) via oral treatment: Toxicity and messenger RNA expression of hemocyte genes[J].Aquatic Toxicology,20093(3):270-277.
[2] Zhang LH;Wu XZ.Capillary electrophoresis with in-capillary solid-phase extraction sample cleanup[J].Analytical chemistry,20076(6):2562-2569.
[3] Zhang LH;Zhang CJ;Chen XM;Feng YQ;Wu XZ.In-capillary solid-phase extraction-capillary electrophoresis for the determination of chlorophenols in water[J].Electrophoresis: The Official Journal of the International Electrophoresis Society,200616(16):3224-3232.
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