Zhou Ying, Du Zhenxia, Zhang Yun
College of Science, Beijing University of Chemical Technology, No. 15 BeiSanhuan East Road, Box 89, 100029 ChaoYang, Beijing, China.
College of Science, Beijing University of Chemical Technology, No. 15 BeiSanhuan East Road, Box 89, 100029 ChaoYang, Beijing, China.
Talanta. 2014 Sep;127:108-15. doi: 10.1016/j.talanta.2014.03.055. Epub 2014 Mar 29.
A simple, highly sensitive and fast procedure for the control of 17 allergenic and prohibited disperse dyes in textile products was optimized. The method was based on ultrasound assisted extraction of textile samples with 10 mL of methanol under controlled conditions (30 min, 70°C). The extracts were analyzed by the ultra-high performance supercritical fluid chromatography (UHPSFC) system coupled with triple quadrupole tandem mass spectrometry (MS/MS). Four stationary phases (BEH, BEH 2-ethyl-pyridine, HSS C18 SB and CSH fluorophenyl) were screened as well as analytical conditions (modifier percentage, backpressure and column temperature) were investigated to improve the separation. All 17 disperse dyes were simultaneously separated and determined by UHPSFC-MS/MS in 5 min. The dyes were monitored via the ESI(+) ionization method and quantified by 3-channel multiple reaction monitoring (MRM). The calibrations were performed and good linear relationship (R≥0.99) was observed within the concentration range of 2-50 μg mL(-1). Satisfactory recoveries (70.55-103.03%) of all the disperse dyes spiked with standards at different levels were demonstrated. This is the first report on the simultaneous analysis of disperse dyes using UHPSFC-MS/MS.
优化了一种用于控制纺织品中17种致敏性和禁用分散染料的简单、高灵敏度且快速的方法。该方法基于在可控条件下（30分钟，70°C）用10毫升甲醇对纺织品样品进行超声辅助萃取。萃取物通过超高效超临界流体色谱（UHPSFC）系统与三重四极杆串联质谱（MS/MS）联用进行分析。筛选了四种固定相（BEH、BEH 2-乙基吡啶、HSS C18 SB和CSH氟苯基），并研究了分析条件（改性剂百分比、背压和柱温）以改善分离效果。所有17种分散染料在5分钟内通过UHPSFC-MS/MS同时分离并测定。染料通过电喷雾电离（ESI(+)）方法进行监测，并通过三通道多反应监测（MRM）进行定量。进行了校准，在2-50微克/毫升的浓度范围内观察到良好的线性关系（R≥0.99）。不同水平添加标准品的所有分散染料均显示出令人满意的回收率（70.55-103.03%）。这是关于使用UHPSFC-MS/MS同时分析分散染料的首次报道。
