建立了基于高效液相色谱-线性离子阱／静电场轨道阱高分辨质谱（ HPLC-LTQ／Orbitrap MS）快速筛查确证生态纺织品中22种禁用分散染料的分析方法。样品在95℃水浴条件下经吡啶／水（1：1，v／v）振荡提取后，以CAPCELL PAK C18色谱柱分离，以乙腈和5 mmol／L乙酸铵（含体积分数为0.01％的甲酸）作为色谱流动相进行梯度洗脱，采用正、负电喷雾（ ESI）离子化模式，利用一级母离子的精确质量数和保留时间对22种分散染料进行快速筛查，利用碰撞诱导解离（ CID）下得到的二级碎片离子进行确证。22种分散染料在各自浓度范围内线性关系良好（ r2>0.99），方法的定量限（ LOQ）为0.125~2.5 mg／kg。除分散黄49外，绝大多数染料在涤纶布、棉涤混纺布两种纺织品基质中的加标回收率在65％~120％之间，相对标准偏差小于15％。应用本方法对涉及多种纤维类型的40余件纺织品样品进行了筛查，其中一个样品检出分散橙37／76。该方法简便、快速，其选择性高，抗干扰性能好，结果准确可靠，可用于纺织品中分散染料的检测。
A rapid screening method based on high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry( HPLC-LTQ/Orbitrap MS)for 22 disperse dyes in ecological textiles has been established. The target compounds were extracted by pyri-dine/water(1:1,v/v)by shaking extraction in 90 ℃ water bath. The extracts were then sepa-rated by a CAPCELL PAK C18 column(100 mm×2. 0 mm,5 μm)using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0. 01%( v/v)formic acid as mobile pha-ses,and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The reten-tion time and accurate mass of parent ion were used for fast screening of 22 disperse dyes, while the confirmatory analysis was obtained by fragments generated by collision-induced disso-ciation(CID)MS/MS. Target analysis exhibited high mass accuracy(<5×10-6). Each target showed a good linearity in its own concentration range and the correlation coefficient was high-er than 0. 99. The LOQs were 0. 125-2. 5 mg/kg. Except for Disperse Yellow 49,the average recoveries of most disperse dyes at three spiked levels were 65%-120%,and the relative stand-ard deviations(n=6)were less than 15%. The method was applied for screening 40 different kinds of textiles,and Disperse Orange 37/76 was detected in one of them. With high selectivity and strong anti-jamming ability,this method is simple,rapid,accurate,and it can be used for the inspection of disperse dyes in textiles.
参考文献
| [1] | García-Lavandeira, J.;Blanco, E.;Salgado, C.;Cela, R..Fast throughput, highly sensitive determination of allergenic disperse dyes in textile products by use of sample composition[J].Talanta: The International Journal of Pure and Applied Analytical Chemistry,20101(1):261-269. |
| [2] | Yang, C.;Zhao, J.;Wang, J.;Yu, H.;Piao, X.;Li, D..Water-based gas purge microsyringe extraction coupled with liquid chromatography for determination of alkylphenols from sea food Laminaria japonica Aresh[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2013:38-42. |
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