单滴微萃取-气相色谱质谱联用法测定纺织品中可分解芳香胺

Determination of aromatic amines from textiles by single drop microextraction combined with gas chromatography

建立了单滴微萃取结合气相色谱一质谱法测定纺织品中可分解芳香胺的方法。研究了萃取剂种类、萃取剂体积、萃取时间、pH和搅拌速度等条件对单滴微萃取效率的影响。确定最佳萃取条件：在室温条件下，取5mL样液，调节被萃取液pH8，以2μL氯苯为萃取剂萃取20min，搅拌速度为200r／min。在优化的实验条件下，检出限为0．08—0．14mg／kg，线性范围0．5～50mg／kg，线性相关系数大于0．996，平均加标回收率为75．3％-96．7％，相对标准偏差为3．6％～8．7％。方法适合纺织品中可分解芳香胺的测定。

A novel method based on single drop microextraetion with gas chromatography-mass spectrometry（ GC- MS） is proposed in this work for determination of aromatic amines in textiles. The effect of experimental variables on the performance of the proposed method, such as extraction solvent, extraction volume, extraction time, pH and stirring speed were investigated. The optimized conditions were obtained： at room temperature, 2 μL of chlorobenzene as single drop extraction solvent,20 min extraction time and 5 mL of aqueous sample （ pH 8 ） at200r/min stirring speed. Under optimized conditions, the linear ranges of 21 aromatic amines were 0. 5 ~ 50 mg/kg detection of limits were 0. 08 ~ 0. 14 mg/kg and the with the correlation coefficients greater than 0. 996. The average recoveries of 21 aromatic amines ranged from 75.3% to 96. 7% with the relative standard deviations between 3.6% and 8.7%. The proposed method has advantages of being quicker and easier to be operated, and lower consumption of organic solvent, and it has been succeesfully applied to the determination of aromatic amines in textile samples.