UPC^2-MS/MS测定烟用纸张中偶氮染料释放的芳香胺  

Determination of aromatic amines released from azo dyes in cigarette paper by UPC^2-MS/MS

作　　者：严俊[1] 周芸[1] 邓惠敏[2] 唐纲岭[2] 李小兰[1] 许蔼飞[1] 杨飞[2] YAN Jun;ZHOU Yun;DENG Huimin;TANG Gangling;LI Xiaolan;XU Aifei;YANG Fei(China Tobacco Guangxi Industrial Co.,Ltd.,Nanning 530001,China;China National Tobacco Quality Supervision ＆ Test Center,Zhengzhou 450001,China)

机构地区：[1]广西中烟工业有限责任公司,南宁市北湖南路28号530001 [2]国家烟草质量监督检验中心

出　　处：《烟草科技》2018年第10期56-63,共8页Tobacco Science & Technology

基　　金：广西中烟工业有限责任公司科技项目"烟用纸张中偶氮染料测定方法研究"(GXZYCX2017C002);国家烟草质量监督检验中心科技创新项目"烟用纸张中偶氮染料的测定方法研究"(562015CA0090)

摘　　要：为测定烟用纸张中偶氮染料释放的芳香胺,通过优化实验条件,建立了一种测定偶氮染料释放的芳香胺的超高效合相色谱-串联质谱(UPC^2-MS/MS)法。样品经连二亚硫酸钠还原、固相萃取净化、C_(18)色谱柱分离后,在多反应监测模式(MRM)下进行MS/MS分析,采用内标法定量。结果表明:(1)各化合物在20～500 ng/mL范围内线性关系良好(R^2>0.99),检出限(LOD)和定量限(LOQ)分别为0.16～0.42和0.51～1.52 mg/kg,除2,4-二氨基甲苯和2,4-二氨基苯甲醚外,其余19种芳香胺的回收率为73.5%～95.0%,相对标准偏差(RSD)<7.0%。(2)采用该方法对30个实际样品进行检测,仅有2个样品在经连二亚硫酸钠还原后检出了部分芳香胺,检测结果与标准方法(GC-MS)结果吻合。该方法分析速度快,分辨率高,溶剂消耗少,适用于烟用纸张中偶氮染料释放的芳香胺的检测。In order to quantify the aromatic amines released from azo dyes from cigarette paper, an ultra-performance convergence chromatography-tandem mass spectrometry（UPC2-MS/MS） method was developed. Sodium dithionite was used to reduce and decompose azo dyes. The extract was analyzed qualitatively and quantitatively by UPC2-MS/MS under multiple reactions monitoring（MRM） mode after purification by solid-phase extraction（SPE） and chromatographic separation by C18 column. The results showed that： 1） Good linear relation was obtained in the range of 20-500 ng/mL for 21 aromatic amines with R2〉0.99.The limits of detection（LODs） and limits of quantification（LOQs） were 0.16-0.42 and 0.51-1.52 mg/kg,respectively. The added standard recoveries of blank samples were in the range of 73.5%-95.0%. The RSDs of most aromatic amines, except 2,4-diaminotoluene and 2,4-diaminoanisole, were less than 7.0%. 2） 30 paper samples were analyzed by the developed method. After reducing by sodium dithionite, aromatic amines were detectable only in two samples, which agreed with the results obtained by a national standard method based on GC-MS. This UPC2-MS/MS method has the advantages of rapid analysis speed, high resolution and low organic reagent consumption, it is suitable for the analysis of 21 aromatic amines released from azo dyes in cigarette paper.

关 键 词：超高效合相色谱-串联质谱法 芳香胺 偶氮染料 烟用纸张 

分 类 号：TS426[农业科学—烟草工业]