A sensitive and efficient procedure for the high throughput determination of banned aromatic amines in textiles and leather products aided by advanced sample composition

A sensitive and efficient procedure for the high throughput determination of banned aromatic amines in textiles and leather products aided by advanced sample composition
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DOI:
10.1007/s00216-010-3574-2
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发表时间:
2010-05-01
影响因子:
4.3
通讯作者:
Cela, R.
Cela, R.
中科院分区:
化学2区
文献类型:
--
作者:
Garcia-Lavandeira, J.;Salgado-Petinal, C.;Cela, R.

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开发并优化了一种高度灵敏的程序,用于对纺织品和皮革产品中禁用偶氮染料衍生的芳香胺进行有效的常规控制。该程序包括按照 EN 14362-1:2003、EN 14362-2:2003 和 ISO/TS 17234:2003 标准中概述的样品制备方案从固体样品中萃取和还原偶氮染料,并使用 Oasis HLB 和 ENVI-Carb 系列吸附剂通过固相萃取净化和浓缩芳香胺。洗脱是通过串联连接的柱进行的,尽管柱的位置颠倒并且ENVI-Carb柱被置于反冲模式。通过液相色谱 (LC)-串联质谱 (MS) 分离和分析萃取和浓缩的芳香胺。色谱分离通过计算机辅助方法开发和专门为 LC-MS 系统开发的特殊化学计量工具(PREGA LC-MS 模块)进行优化。该系统可以在几次启动等度和梯度实验后实现无人值守的分离优化。优化的分离程序能够以非常低的定量限准确检测和测量所考虑的所有 23 种芳香胺,并且没有任何显着的基质效应。战略性样品组合被用作降低纺织品和皮革制品中芳香胺控制成本和工作量的有效手段。通过 20 个样本的案例研究证明了战略样本组成的好处。
A highly sensitive procedure for the efficient routine control of aromatic amines derived from banned azo dyes in textile and leather products was developed and optimized. The procedure involves the extraction and reduction of azo dyes from solid samples following the sample preparation protocols outlined in EN 14362-1:2003, EN 14362-2:2003, and ISO/TS 17234:2003 standards, and cleanup and concentration of aromatic amines by solid-phase extraction, with Oasis HLB and ENVI-Carb sorbents in series. The elution was carried out with the cartridges connected in series, although the positions of the cartridges were reversed and the ENVI-Carb cartridge was placed in the backflush mode. Extracted and concentrated aromatic amines were separated and analyzed by liquid chromatography (LC)-tandem mass spectrometry (MS). The chromatographic separation was optimized by means of computer-assisted method development with a special chemometric tool (the PREGA LC-MS module), developed specifically for LC-MS systems. This system enables the unattended optimization of separations after a few priming isocratic and gradient experiments. The optimized separation program enables accurate detection and measurement of all the 23 aromatic amines considered, at very low quantification limits and without any notable matrix effects. Strategic sample composition was applied as an efficient means of reducing the costs and work involved in the control of aromatic amines in finished textile and leather products. The benefits of strategic sample composition are demonstrated by means of a case study of 20 sample specimens.