色谱

色谱 ›› 2015, Vol. 33 ›› Issue (1): 68-74.DOI: 10.3724/SP.J.1123.2014.09023

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定纺织助剂中双(氢化牛脂基)二甲基季铵化合物

朱峰1,2   

  1. 1. 国家纺织服装产品质量监督检验中心(福建), 福建 福州 350026;
    2. 福建省纤维检验局, 福建 福州 350026
  • 收稿日期:2014-09-17 修回日期:2014-10-29 出版日期:2015-01-08 发布日期:2014-12-26
  • 通讯作者: 朱峰
  • 基金资助:

    福建省质量技术监督局科技项目(FJQI2012003).

Determination of di(hydrogenated tallow alkyl) dimethyl ammonium compounds in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry

ZHU Feng1,2   

  1. 1. National Textile and Garment Quality Supervision Testing Center (Fujian), Fuzhou 350026, China;
    2. Fujian Fiber Inspection Bureau, Fuzhou 350026, China
  • Received:2014-09-17 Revised:2014-10-29 Online:2015-01-08 Published:2014-12-26

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200

被引次数

1

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, 1.8 μm)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10~280 μg/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.

关键词: 超高效液相色谱-串联质谱, 纺织助剂, 双(氢化牛脂基)二甲基季铵化合物

Abstract:

A method has been developed for the determination of di(hydrogenated tallow alkyl) dimethyl ammonium compounds (DHTDMAC) in textile auxiliaries by ultra-high performance 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. Identification 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 indicated 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 0.9991. 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.

Key words: di(hydrogenated tallow alkyl) dimethyl ammonium compounds (DHTDMAC), textile auxiliaries, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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