摘要
建立了快速测定纺织助剂中双（氢化牛脂基）二甲基季铵化合物（ DHTDMAC）的超高效液相色谱-串联质谱（UPLC-MS／MS）分析方法。样品经5％（v／v）甲酸甲醇超声波提取、稀释后，采用Eclipse Plus C18柱（50 mm×2.1 mm，1.8μm）分离，甲醇和0.1％（ v／v）甲酸水溶液为流动相梯度洗脱，电喷雾离子源正离子多反应监测模式进行定性和定量分析。实验结果表明，DHTDMAC在10-280μg／L范围内与峰面积呈良好的线性关系，相关系数（ r2）为0.9991；以不低于3倍信噪比计算方法检出限（ LOD，S／N=3）为3 mg／kg；方法定量限（ LOQ，S／N=10）为10 mg／kg。3种纺织助剂基质中 DHTDMAC 在3个不同加标水平的平均回收率为97.2％-108.3％，相对标准偏差（ RSD）为1.5％-4.6％。该方法灵敏度高、操作简便、快速准确，适用于纺织助剂中 DHTDMAC的分析测定。
A method has been developed for the determination of di（ hydrogenated tallow alkyl）dimethyl ammonium compounds（ DHTDMAC ） in textile auxiliaries by ultra-high per-formance liquid chromatography-tandem mass spectrometry （ UPLC-MS/MS ）. The samples were extracted and diluted with acidified methanol by 5%（ v/v）formic acid under ultrasonic assistance. The separation was performed on an Eclipse Plus C18 column（ 50 mm ×2. 1 mm, 1. 8 μm）using 0. 1%（ v/v）formic acid solution and methanol as the mobile phases. Identifica-tion and quantification were achieved by UPLC-MS/MS with electrospray ionization （ ESI ） source in positive ion mode and multiple reaction monitoring（ MRM）mode. The results indica-ted that the calibration curve of DHTDMAC showed good linear relationship between peak area and mass concentration in the range of 10-280 μg/L with the correlation coefficient（ r2）of 0. 999 1. The limit of detection（ LOD,S/N=3）and the limit of quantification（ LOQ,S/N=10） of this method were 3 mg/kg and 10 mg/kg,respectively. The average recoveries from three typical textile auxiliary matrices including dispersant,anti-static agent and fabric softener,at three spiked levels were in the range of 97. 2%-108. 3% with the relative standard deviations （ RSDs）of 1. 5%-4. 6%. The method is sensitive,accurate,simple and effective for the analysis of DHTDMAC in textile auxiliaries.
出处
《色谱》
CAS
CSCD
北大核心
2015年第1期68-74,共7页
Chinese Journal of Chromatography
基金
福建省质量技术监督局科技项目(FJQI2012003)
关键词
超高效液相色谱-串联质谱
双(氢化牛脂基)二甲基季铵化合物
纺织助剂
ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）
di （ hydrogenated tallow alkyl） dimethyl ammonium compounds （ DHTDMAC ）
textile auxiliaries
作者简介
通讯联系人．Tel：（0591）83595610，E-mail：zhufengdr@163．com
