Niu Zengyuan, Luo Xin, Ye Xiwen, Xiu Xiaoli, Zhang Li, Wang Xin, Chen Jing
Se Pu. 2015 Oct;33(10):1104-9. doi: 10.3724/sp.j.1123.2015.04048.
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 pyridine/water (1:1, v/v) by shaking extraction in 90 degrees C water bath. The extracts were then separated by a CAPCELL PAK C18 column (100 mm x 2.0 mm, 5 μm) using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0.01% (v/v) formic acid as mobile phases, and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The retention 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 dissociation (CID) MS/MS. Target analysis exhibited high mass accuracy (< 5 x 10(-6)). Each target showed a good linearity in its own concentration range and the correlation coefficient was higher 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 standard 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.
建立了一种基于高效液相色谱 - 线性离子阱/轨道阱高分辨率质谱(HPLC-LTQ/Orbitrap MS)的生态纺织品中22种分散染料快速筛选方法。目标化合物采用吡啶/水(1:1,v/v)在90℃水浴中振荡萃取。萃取液随后通过CAPCELL PAK C18柱(100 mm×2.0 mm,5μm)进行分离,以乙腈 - 含0.01%(v/v)甲酸的5 mmol/L醋酸铵为流动相进行梯度洗脱,最后采用HPLC-LTQ/Orbitrap在正、负离子电喷雾电离(ESI)模式下进行分析。利用保留时间和母离子精确质量对22种分散染料进行快速筛选,同时通过碰撞诱导解离(CID)串联质谱(MS/MS)产生的碎片进行确证分析。目标分析显示出高的质量准确度(<5×10⁻⁶)。各目标物在其自身浓度范围内呈现良好的线性,相关系数高于0.99。定量限为0.125 - 2.5 mg/kg。除分散黄49外,大多数分散染料在三个加标水平下的平均回收率为65% - 120%,相对标准偏差(n = 6)小于15%。该方法应用于40种不同纺织品的筛选,其中一种检测出了分散橙37/76。该方法具有高选择性和强抗干扰能力,操作简单、快速、准确,可用于纺织品中分散染料的检测。