色谱

色谱

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基于氨基柱的反相/正相液相色谱-电喷雾串联质谱法测定纺织品中的二硬脂基二甲基氯化铵

丁友超1, 申晓萍2, 吴晓琼3, 吴丽娜1, 曹锡忠1*   

  1. 1. 江苏出入境检验检疫局工业产品检测中心, 江苏 南京 210001; 2. 南通出入境检验检疫局综合技术中心, 江苏 南通 226005; 3. 南京化工职业技术学院应用化学系, 江苏 南京 210048
  • 收稿日期:2011-02-21 修回日期:2011-03-15 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 曹锡忠,研究员,主要从事生态纺织品检测和认证研究. Tel: (025)52345242,
  • 基金资助:

    “十一五”国家科技支撑计划重点项目;质检公益性行业科研专项项目

Determination of distearyl dimethyl ammonium chloride in textiles by reversed-phase and normal-phase liquid chromatography-electrospray ionizationtandem mass spectrometry

DING Youchao1, SHEN Xiaoping2, WU Xiaoqiong3, WU Lina1, CAO Xizhong1*   

  1. 1. Inspection Center of Industry Products, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2. Poly-technology Center, Nantong Entry-Exit Inspection and Quarantine Bureau, Nantong 226005, China; 3. Department of Applied Chemistry, Nanjing Chemical Engineering Polytechnic College, Nanjing 210048, China
  • Received:2011-02-21 Revised:2011-03-15 Online:2011-06-28 Published:2011-07-25

PDF

584

被引次数

14

摘要： 建立了纺织品中二硬酯基二甲基氯化铵(DSDMAC)的反相(RP)/正相(NP)液相色谱-电喷雾串联四极杆质谱(LC-ESI-MS/MS)的分析方法。选用甲醇为提取溶剂,确定了超声功率为420 W、提取温度为70 ℃的超声波辅助提取条件,实现了30 min快速提取样品中的DSDMAC。建立了基于氨基柱的反相和正相两套液相色谱分离系统,采用LC-MS/MS的选择反应监测(SRM)模式检测3个DSDMAC组分。结果显示: RPLC和NPLC对DSDMAC的检出限(S/N=3)分别为0.1 mg/kg和0.01 mg/kg。采用RPLC-MS/MS为定量方法,对8种不同的空白纤维纺织品的添加回收率为85.5%～103%(n=5);平行测试的相对标准偏差(RSD)为4.18%～12.8%(n=5)。5家外部实验室分别采用上述方法对2种参考样品中的DSDMAC进行检测,实验室间测定的RSD分别为7.3%和9.4%。该方法快速、准确、稳定,适用于纺织品中DSDMAC的检测。

关键词: 二硬酯基二甲基氯化铵, 反相/正相液相色谱, 纺织品, 季铵盐化合物, 液相色谱-串联质谱

Abstract: A method of reversed-phase (RP)/normal-phase (NP)-liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was developed for the determination of distearyl dimethyl ammonium chloride (DSDMAC) in textiles. The DSDMAC in textile was extracted by ultrasound-assisted extraction using methanol as extraction solvent under the conditions of 70 ℃ and 420 W within 30 min. The three quaternary ammonium compounds of DSDMAC were detected by LC-MS/MS in the selective reaction monitoring (SRM) mode. The limits of detection (LODs) (S/N=3) of DSDMAC detected by RPLC-MS/MS and NPLC-MS/MS based on an amino-column were 0.1 mg/kg and 0.01 mg/kg, respectively. The recoveries of DSDMAC spiked in the eight different types of blank fabrics ranged from 85.5% to 103% with the relative standard deviations (RSDs) of 4.18%~12.8% (n=5) by RPLC-MS/MS method. Five laboratories were invited to take part in the validation of the method, and the RSDs of inter-lab were 7.3%~9.4% on two reference samples. The method is fast, accurate and reproducible, and can meet the demands of the determination of DSDMAC in textiles.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), textiles, distearyl dimethyl ammonium chloride (DSDMAC), quaternary ammonium compounds, reversed-phase/normal-phase liquid chromatography (RPLC/NPLC)