气相色谱-质谱法检测纺织品中28种芳香胺和4种芳香胺盐  

Determination of 28 aromatic amines and 4 aromatic amine salts in textiles by gas chromatography-mass spectrometry

作　　者：刘金源 叶曦雯 罗忻 牛增元 刘坤 陈静 李晶莹[1] LIU Jinyuan;YE Xiwen;LUO Xin;NIU Zengyuan;LIU Kun;CHEN Jing;LI Jingying(College of Environmental and Safety Engineering,Qingdao University of Science and Technology,Qingdao 266042,China;Technology Center of Qingdao Customs,Qingdao 266109,China)

机构地区：[1]青岛科技大学环境与安全工程学院,青岛266042 [2]青岛海关技术中心,青岛266109

出　　处：《分析试验室》2023年第12期1591-1598,共8页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(NQI2016YFF0203702);海关总署科研项目(2019HK070)资助。

摘　　要：建立了同时测定纺织品中28种芳香胺和4种芳香胺盐的气相色谱-质谱方法。纺织品样品中偶氮染料和游离态的芳香胺盐在碱性的柠檬酸盐缓冲溶液中,经连二亚硫酸钠还原成芳香胺,经叔丁基甲醚溶剂提取,气相色谱-质谱法同时测定。优化条件为2 mL质量分数40%的NaOH碱化、10 mL叔丁基甲醚提取。28种芳香胺均呈良好的线性关系,26种芳香胺线性范围为0.05~10 mg/L,2,4-二氨基苯甲醚和2,5-二氨基甲苯的线性范围为0.2~10 mg/L;相关系数为0.996~0.999;26种芳香胺检出限为0.05 mg/L,2,4-二氨基苯甲醚和2,5-二氨基甲苯的检出限为0.2 mg/L。2,4-二氨基苯甲醚硫酸盐的加标回收率为33.1%~36.0%,其余3种芳香胺盐平均加标回收率为84.5%~124.6%;2,4-二氨基苯甲醚加标回收率为43.7%~64.3%,其余27种芳香胺回收率在71.7%~119.3%之间。阳性样品检测结果表明:对于原有芳香胺化合物的检测,本方法和ISO 14362方法对比无显著差异;对新增芳香胺特别是2,5-二氨基甲苯,ISO 14362方法存在漏检风险,而本方法具有更高的回收率。本方法为OEKO-TEX新增的芳香胺及芳香胺盐的检测提供了参考。A method for the detection of 28 aromatic amines and 4 aromatic amine salts in textiles by gas chromatography-mass spectrometry was established.Azo dyes and free aromatic amine salts in textiles were reduced to aromatic amines by sodium dithionite in alkaline citrate buffer solution,extracted by tert-butyl methyl ether solvent,and then determined simultaneously by gas chromatography-mass spectrometry.The optimized pretreatment conditions were alkalized by 2 mL of 40%NaOH and extracted by 10 mL of tert butyl methyl ether.28 aromatic amines showed good linear relationships,the linear ranges were 0.05-10 mg/L for 26 aromatic amines,and 0.2-10 mg/L for 2,4-diaminoanisole and 2,5-diaminotoluene,with the correlation coefficients of 0.996-0.999.The detection limits were 0.05 mg/L for 26 aromatic amines,and 0.2 mg/L for 2,4 diaminoanisole and 2,5-diaminotoluene.The standard adding recovery experiments showed that the recoveries of 2,4-diaminoanisole sulfate were 33.1%-36.0%,and that of the other three aromatic amine salts were 84.5%-124.6%.The recoveries of 2,4-diaminoanisole were 43.7%-64.3%,and that of the other 27 aromatic amine were 71.7%-119.3%.The test results of positive samples showed that there was no significant difference between this method and ISO 14362 method for the detection of original aromatic amine compounds.For newly added aromatic amines,especially 2,5-diaminotoluene,the ISO 14362 method has the risk of missing detection,while this method has a higher recovery rate,and can provide a reference for the detection of newly added aromatic amines and aromatic amine salts in OEKO-TEX.

关 键 词：气相色谱-质谱法 芳香胺 芳香胺盐 纺织品 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]