涤纶中致癌芳香胺的加速溶剂萃取-UPLC-MS/MS快速测定  

Determination of aromatic amines in terylene by ASE coupled with UPLC-MS /MS

作　　者：吴刚 王力君 张明誉 郭方龙 赵珊红 

机构地区：[1]浙江省检验检疫科学技术研究院,浙江杭州310015 [2]浙江立德产品技术有限公司,浙江杭州310015

出　　处：《纺织学报》2014年第7期94-100,共7页Journal of Textile Research

基　　金：国家质检总局科研项目(2011IK110);浙江省科技厅公益性资助项目(2011C21064)

摘　　要：利用加速溶剂萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)技术,建立了一种能在6 min内快速分离和测定涤纶中禁用偶氮染色剂可分解出的22种致癌芳香胺的方法。样品经丙酮加速溶剂萃取、浓缩,再经氧化-还原裂解反应,乙酸乙酯萃取,N2吹至近干后,用甲醇/水溶液(体积比1/9)溶解,采用Acquity UPLCBEH C18柱,以甲醇-0.05%甲酸溶液为流动相,梯度洗脱,电喷雾正离子模式电离,多反应监测模式检测,外标法定量。该方法检出限(LOD)为0.96~17.0μg/kg,定量限(LOQ)为3.2~56.1μg/kg;在0.01~0.2μg/mL范围内线性关系良好,添加浓度分别为5.0,10.0,15.0 mg/kg时,添加回收率范围为(33.28±1.83)%^(107.14±1.10)%,相对标准偏差为0.38%~10.9%。A novel method has been developed for rapid separation and determination of 22 kinds of aromatic amines derived from banned azo colorants in terylene by accelerated solvent extraction（ ASE）with acetone coupled with ultra performance liquid chromatography-tandem mass spectrometry（ UPLCMS /MS） in 6 min. The colorants in terylene were extracted by ASE with acetone. The extract was condensed,then subjected to REDOX cracking reaction,and then ethyl acetate was used to extract aromatic amines from the reaction liquid. The extract was blowed with N2to nearly dry,and redissolved in the solvent of methanol and water（ 1 /9,v /v）. The chromatographic analysis was performed on an Acquity UPLC BEH C18column by a gradient elution employing methanol and 0. 05% formic acid as a mobile phase. The analytes were detected using electrospray ionization（ ESI） tandem mass spectrometry with multiple reaction monitoring（ MRM） in positive ion mode. The calibration curves showed good linearity in the range of 0. 01- 0. 2 μg /mL for all compounds with the limits of determination（ LOD） of0. 96- 17. 0 μg /kg,and the limits of quantification（ LOQ） of 3. 2- 56. 1 μg /kg. The recoveries of 22kinds of aromatic amines at the spiked concentration levels of 5. 0,10. 0 and 15. 0 mg /kg ranged from（ 33. 28 ±1.83） % to（ 107.14 ±1. 10） % with relative standard deviations（ RSDs） of 0.38%-10.9%（ n =6）.

关 键 词：加速溶剂萃取 超高效液相色谱-串联质谱 涤纶 禁用偶氮染料 

分 类 号：O652.1[理学—分析化学]