纺织品中有害有机溶剂的快速筛查和确证  

Rapid screening and confirmation of harmful organic solvents in textiles

作　　者：谢堂堂[1] 王成云[1] 潘晓远 马婷[1] 林君峰[1] 

机构地区：[1]深圳出入境检验检疫局工业品检测技术中心,广东深圳518067

出　　处：《印染》2017年第14期40-46,共7页China Dyeing and Finishing

基　　金：国家质检总局科研项目(2012IK119;2014IK163)

摘　　要：建立了快速筛查和确证纺织品中有害有机溶剂残留量的液质联用方法。该方法以甲醇为萃取溶剂,超声萃取纺织品中残留的有害有机溶剂;萃取液直接进行超高效液相色谱/静电场轨道阱高分辨质谱分析,根据提取离子色谱峰面积进行外标法定量。采用Hypersil GOLD色谱柱对20种有害有机溶剂进行色谱分离,以甲醇/水为流动相,梯度洗脱。质谱分析采用电喷雾正离子(ESI+)模式,一级质谱全扫描范围为m/z 50~300,根据保留时间和准分子离子精确质量数进行定性,根据二级质谱进行确证。该方法的定量限为0.5~10.0μg/kg,平均加标回收率为82.3%~94.9%,相对标准偏差为4.2%~10.7%。该方法简便快速、灵敏度高,定量限远低于REACH法规的要求。An effective method is established for the rapid screening and confirmation of residual organic solvents in textiles. Residual harmful organic solvents are ultrasonically extracted with methanol as an extraction solvent. The extract is then analyzed by ultra-high performance liquid chromatography/orbi- trap high resolution mass spectrometry （UPLC/Orbitrap HRMS）. The quantitative analysis is carried out by the peak area in extracted chromatography and the concentration of each analyte is calibrated by the external standard method. The chromatographic separation of twenty harmful organic solvents is per- formed on an Hypersil GOLD column with a gradient elution of methanol/water. The mass spectrometry analysis is carried out by orbitrap high resolution mass spectrometry in ESI＋ mode with full-scan experi- ment in range of m/z 50-300. The qualitative analysis is carried out by the retention time and the accu- rate mass of quasi-molecular ion, and the confirmation is carried out by the daughter ions in ddMS2 mode. The limits of quantification （LOQs） varies from 0.5 μg/kg to 10.0 μg/kg, the average spiked recov- eries changes from 82.3% to 94.9% while the relative standard deviation （RSD） is 4.2%-10.7%. The pro- posed method is simple, rapid and sensitive with LOQs far less than the limited requirements of REACH.

关 键 词：测试 有害有机溶剂 超高效液相色谱 静电场轨道阱高分辨质谱 筛查 确证 纺织品 

分 类 号：TS107[轻工技术与工程—纺织工程]