摘要
针对纺织品中联苯胺测定时样品前处理存在的问题,对纺织品中联苯胺检测方法中的样品前处理条件进行了研究探讨。采用气相色谱-质谱（GC/MS）分析技术,DB-5 MS石英毛细管柱,选择离子检测（SIM）模式,选择特征碎片离子（m/z）184对联苯胺含量进行检测。对前处理条件中检测结果有明显影响的因素：提取溶剂的选择,还原剂连二亚硫酸钠溶液的配制时间,放置时间和光照等条件进行了考察。解决了由于前处理操作差别带来的联苯胺回收率偏低的问题,提高了检测的准确度和效率。联苯胺质量浓度在0.1~30 mg/L范围内线性关系良好,线性相关系数为r2=0.9993,检出限为1.0 mg/kg,回收率在85%~108%之间。
A method for the determination of benzidine in textiles using GC-MS in SIM mode was developed, and the research on the pretreatment conditions was fully conducted. The DB-5 MS capillary column was used as a chromatographic column, while the characteristic ion of m/z 184 was selected as the quantitative ion for benzidine. Mainly Influencing factors such as the selection of extraction solvent and storage condition of the sodium dithionite solution were discussed in detail. Obstacles of the relatively low recovery due to the pretreatment condition could be overcome and the accuracy and efficiency could also be enhanced. The linear range was 0. 1-30 mg/L with the correlation coefficient of 0. 9993, and the average recoveries were in the range of 85% - 108% with a detection limit as low as 1.0 mg/kg. The method has been applied to the determination of benzidine in textiles with satisfactory results.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第10期1225-1228,共4页
Chinese Journal of Analysis Laboratory
关键词
气相色谱-质谱
联苯胺
纺织品
影响因素
Gas chromatography-mass spectrometry
Benzidine
Textiles
Pretreatment condition
