纺织学报 ›› 2020, Vol. 41 ›› Issue (08): 69-73.doi: 10. 13475/ j.fzxb.20190904906

• 染整与化学品 • 上一篇    下一篇

用气相色谱-质谱法测定纺织柔软剂中的环硅氧烷

于 岩1,2, 章若红2, 钟 毅1, 杜英英2, 毛志平1, 徐 红1   

  1. 1. 东华大学生态纺织教育部重点实验室, 上海 201620;  2. 上海市质量监督检验技术研究院, 上海 201114
  • 收稿日期:2019-09-18 修回日期:2020-05-22 出版日期:2020-08-15 发布日期:2020-08-21

Determination of cyclicsilicates in textile softeners by gas chromatography-mass spectrometry

YU Yan1,2, ZHANG Ruohong2, ZHONG Yi1, DU Yingying2, MAO Zhiping1, XU Hong1   

  1. 1. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China;  2. Shanghai Institute of Quality Inspection and Technical Research, Shanghai 201114, China
  • Received:2019-09-18 Revised:2020-05-22 Online:2020-08-15 Published:2020-08-21

摘要:

为开发纺织柔软剂中环硅氧烷高效定量分析方法,建立了气相色谱-质谱(GC-MS)联用测定纺织柔软剂中环硅氧烷的分析方法。利用乙酸乙酯作为提取溶剂对样品进行振荡提取,并将提取的溶液经过滤后与六甲基二硅氮烷进行衍生化反应,反应后的溶液采用GC-MS 进行检测。结果表明:在混合标准溶液质量浓度为1 ~ 100 mg/ L 范围内,GC-MS 法测定八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)的峰面积与混合标准溶液质量浓度具有良好的线性关系,相关系数R2 ≥ 0. 995 3;GC-MS 法的检出限为0. 117 0~0. 201 0 mg/ L, 定量限为0. 390 0~0. 670 0 mg/ L,重复性和稳定性相对标准偏差分别小于1. 0%和7. 4%,样品加标回收率为89. 8%~114. 3%,相对标准偏差为1. 3%~6. 4%,满足检测的要求;GC-MS 法的操作简单,可精准地检测出纺织柔软剂中D4、D5、D6 的微量残留。

关键词: 气相色谱-质谱联用法, 纺织柔软剂, 环硅氧烷测定, 八甲基环四硅氧烷, 十甲基环五硅氧烷, 十二甲基环六硅氧烷

Abstract:

In order to develop an efficient quantitative analysis method on the content of cyclosiloxane in textile softener, gas chromatography-mass spectrometry ( GC-MS) was carried out to establish an analytical method for this purpose. The test sample was extracted by the oscillating extraction method using ethyl acetate as the solvent. The extracted solution was subjected to a derivatization reaction with hexamethyldisilazane, and then was detected using GC-MS. The result shows that within range of solution mass density 1 - 100 mg/ L, the peak areas measured for octamethylcyclotetrasiloxane ( D4 ), decamethylcyclopentasiloxane(D5) and dodecamethylcyclohexasiloxane (D6) demonstrate good linear relationship with solution mass density, with correlation coefficient R2≥ 0. 995 3. The detection limit of this method is 0. 117 0-0. 201 0 mg/ L, the limit of quantification is 0. 390 0-0. 670 0 mg/ L, the relative standard deviation ( RSD) of repeatability and stability are less than 1. 0% and 7. 4% respectively. The sample recovery rate is 89. 8%-114. 3%, and the RSD is 1. 3%-6. 4%, satisfying the testing requirements. This method is easy to operate and capable of determining with accuracy the trace residues of D4, D5 and D6 in textile softeners.

Key words: gas chromatography-mass spectrometry, textile softener, cyclosiloxane determination, octamethylcyclote-trasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane

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