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分散固相萃取/气相色谱-三重四极杆串联质谱法检测纸张中的20种芳香胺
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周培琛,梁晖,邓其馨,张建平,黄延俊,黄华发,刘泽春,刘江生,许寒春,谢卫 福建中烟工业有限责任公司技术中心 
基金项目:福建中烟工业有限责任公司技术中心科技项目(ZX2017008)
中文摘要:建立了纸张中的20种芳香胺的分散固相萃取/气相色谱-三重四极杆串联质谱分析方法。纸张中的偶氮染料于(70±2)℃经预处理后还原为芳香胺,向反应后的悬浮液中先加入4 mL 10 mol/L氢氧化钠溶液,将pH值由弱酸性调至碱性,再加入0.5 mL的3内标(氘代萘、2,4,5-三氯苯胺和氘代蒽)工作溶液、10 mL的叔丁基甲醚,最后加入15 g无水硫酸钠除水,振摇40 min萃取芳香胺。萃取液经分散固相萃取试剂盒(d-SPE)进一步净化、离心后,取上层清液以气相色谱-三重四极杆串联质谱法(GC-MS/MS),在多反应离子监测(MRM)模式下检测,内标法定量。目标物在各自浓度范围内线性关系良好(r2>0.99),在10、20、50 ng/mL 3个加标水平下的回收率为80.7%~128%,相对标准偏差(RSDs)为0.79%~6.5%,检出限(LOD)为0.05~2.1 ng/mL,定量下限(LOQ)为0.18~5.5 ng/mL。该方法简便快捷,灵敏度高,可用于纸张中芳香胺的快速检测。
中文关键词:分散固相萃取(d-SPE)  气相色谱-三重四极杆串联质谱法(GC-MS/MS)  芳香胺  纸张
 
Determination of 20 Aromatic Amines in Paper by Dispersive Solid Phase Extraction/Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry
Abstract:A gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS) with dispersive solid phase extraction(d-SPE) was developed for the determination of azo colorants in paper.The azo colorants were reduced as aromatic amines after pretreatment.Sequentially,4 mL 10 mol/L sodium hydroxide solution,0.5 mL three internal standards(naphthalene-D8,2,4,5-trichloro-aniline and anthracene-D10)working solution,10 mL tert-butyl methyl ether and 15 g anhydrous sodium sulfate were added into the suspension to adjust the pH value from faintly acid to alkaline and absorb water.The aromatic amines were extracted with 10 mL tert-butyl methyl ether via 40 min thorough oscillation.The extract was further purified with d-SPE kits.After centrifugation,the supernatant was determined by GC-MS/MS in highly sensitive and selective multiple reaction monitoring mode(MRM),and quantified by internal standard method.There existed good linear relationships for the target compounds in respective concentration ranges,with their correlation coefficients(r2) larger than 0.99.The recoveries at three spiked levels of 10,20 and 50 ng/mL were between 80.7% and 128%,with the relative standard deviations(RSDs) of 0.79%-6.5%.The limits of detection(LODs) and limits of quantification(LOQs) were in the ranges of 0.05-2.1 ng/mL and 0.18-5.5 ng/mL,respectively.Results showed that the method was simple,rapid and sensitive,was applicable for the rapid detection of aromatic amines in paper.
Key Words:dispersed solid phase extraction(d-SPE)  gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)  aromatic amines  paper
引用本文:周培琛,梁晖,邓其馨,张建平,黄延俊,黄华发,刘泽春,刘江生,许寒春,谢卫.分散固相萃取/气相色谱-三重四极杆串联质谱法检测纸张中的20种芳香胺[J].分析测试学报,2019,(6):718-723.
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