色谱

色谱 ›› 2011, Vol. 29 ›› Issue (04): 353-357.DOI: 10.3724/SP.J.1123.2011.00353

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定纺织助剂中的有机锡

李艳明1, 胡勇杰2*, 刘金华1, 郭玉良1, 王桂琴1   

  1. 1. 广东德美精细化工股份有限公司, 广东 顺德 528305; 2. 广东产品质量监督检验研究院, 广东 广州 510308
  • 收稿日期:2010-12-16 修回日期:2011-02-24 出版日期:2011-04-28 发布日期:2011-04-28
  • 通讯作者: 胡勇杰,工程师,研究方向为纺织服装及纺织助剂分析检测. Tel: (020)89232286, E-mail: huyongjie520@sohu.com.
  • 基金资助:
    2008年广东省地方标准制订计划项目(粤质监函［2008］354号).

Determination of organotin compounds in textile auxiliaries by gas chromatography-mass spectrometry

LI Yanming1, HU Yongjie2*, LIU Jinhua1, GUO Yuliang1, WANG Guiqin1   

  1. 1. Dymatic Chemicals, Inc., Shunde 528305, China; 2. Guangdong Testing Institute of Product Quality Supervision, Guangzhou 510308, China
  • Received:2010-12-16 Revised:2011-02-24 Online:2011-04-28 Published:2011-04-28
  • Contact: Yanming LI

PDF

798

摘要： 建立了纺织助剂中二丁基锡(dibutyltin, DBT)、三丁基锡(tributyltin, TBT)及三苯基锡(triphenyltin, TPhT)化合物的气相色谱-质谱联用(gas chromatography-mass spectrometry, GC-MS)检测方法。在乙酸-乙酸钠缓冲溶液(pH 4.0)中,用正己烷超声萃取(对疏水性样品)或振荡萃取(对亲水性样品)试样中的有机锡,然后以四乙基硼化钠的四氢呋喃溶液为衍生化试剂进行衍生化,用GC-MS测定,依据保留时间和选择离子定性,外标法定量。实验结果表明,在0.1～8.0 mg/L(对于DBT和TBT)或0.1～4.0 mg/L(对于TPhT)的范围内,有机锡化合物的浓度（以有机锡阳离子计）与其衍生物峰面积呈良好的线性关系,线性相关系数(r2)为0.9994～0.9998,检出限为0.003～0.005 mg/L; 4种聚氨酯类助剂基质中3种有机锡化合物的平均加标回收率为92.6%～108.0%,相对标准偏差为2.5%～10.2%。该方法的技术指标满足纺织助剂中有机锡化合物的测定要求。

关键词: 纺织助剂, 气相色谱-质谱法, 有机锡

Abstract: A gas chromatography-mass spectrometry (GC-MS) method has been developed for the determination of dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPhT) in textile auxiliaries. The sample was first extracted with n-hexane in acetate buffer solution (pH 4.0) under ultrasonication (for hydrophobic sample) or oscillation extraction (for hydrophilic sample) and then derivatized with sodium tetraethylborate in tetrahydrofuran. The derivative was determined by GC-MS in selected ion monitoring (SIM) mode. The separation and quantification were achieved using a Rxi-5ms silica capillary column (30 m×0.25 mm×0.25 μm). The linear ranges were 0.1~8.0 mg/L for both DBT and TBT, and 0.1~4.0 mg/L for TPhT. There were good linear relationships between the peak area and concentration in the linear ranges and the correlation coefficients (r2) were 0.9994~0.9998. The detection limits (LOD) were from 0.003 mg/L to 0.005 mg/L. The average recoveries of these organotin compounds at the three spiked levels of 4.0, 10.0 and 40.0 mg/kg were 92.6%~108.0% with the relative standard deviations (RSDs) of 2.5%~10.2%. The method is simple and accurate for simultaneous analysis of the DBT, TBT and TPhT in textile auxiliaries.

Key words: gas chromatography-mass spectrometry (GC-MS), organotin, textile auxiliary