材料期刊网

建立了同时测定染发剂中4，4′-二氨基二苯胺硫酸盐和2，4-二氨基苯酚硫酸盐等6种染料的超高效液相色谱-串联质谱（UPLC-MS／MS）分析方法。以水为提取剂进行超声提取，用 Waters BEH-C18柱（100 mm×2.1 mm，1.7μm）分离，以10 mmol／L的乙酸铵和乙腈为流动相进行梯度洗脱。在电喷雾正离子模式下，采用多反应监测（MRM）模式进行定性和定量分析。6种染料在相应的质量浓度范围内线性关系良好，线性相关系数（R2）均大于0.99，检出限为0.26~4.6 mg／kg，回收率为83.0％~92.2％，相对标准偏差为5.4％~11.2％。方法精密度、准确度、回收率和基质效应均符合染发剂样品测定的要求，用于实际样品测定，结果满意。本方法准确、简便、快速，适用于染发剂中6种染料的分析测定。

A sensitive method was developed for the simultaneous determination of six compo-nents which included 4,4′-diaminodiphenylamine sulfate hydrate and 2,4-diaminophenol sul-fate,etc. in hair dyes by ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS). After extracted by water through ultrasonic extraction,the samples were ana-lyzed by UPLC-MS/MS. The separation was performed on a Waters BEH-C 18 column( 100 mm × 2. 1 mm,1. 7 μm)with gradient elution of 10 mmol/L ammonium acetate and acetonitrile. The electrospray ionization( ESI)source in positive ion mode was used for the analysis of the six components in the multiple reaction monitoring( MRM)mode. The results showed good linear relationships with all the correlation coefficients(R2)more than 0. 99. The limits of detection (LODs,S/N=3)for the six components were in the range of 0. 26-4. 6 mg/kg. The average recoveries of the six components in the spiked samples were in the range of 83. 0%-92. 2% with the relative standard deviations( RSDs,n=6)of 5. 4%-11. 2%. The precision,accuracy,mean recoveries and the matrix effects satisfied the requirements of cosmetic sample measurement. The proposed method has been applied to the determination of six dyes in actual samples. This method is simple,accurate and effective for the simultaneous determination of the six compo-nents in hair dyes.