丝织物中酸性金黄G的液相色谱-质谱法测定

Determination of Metanil Yellow G in silk fabric by liquid chromatography tandem mass spectrometry

建立了固相萃取一超快速液相色谱一电喷雾串联三重四级质谱（SPE—UFLC—ESI—MS／MS）联用技术测定丝织物中的酸性金黄G。样品经SPE提取和净化后，采用ACQUITY UPLC BEH C18柱（100mm×2．1mm,1．7μm）色谱柱，乙腈（含0．1％甲酸）和水（含0．1％甲酸）为流动相进行梯度洗脱，电喷雾离子源电离，负离子多反应监测模式进行定性定量分析。酸性金黄G染料在0．5-100．0μg／L范同内线性良好，相关系数0．9995，方法检出限为0．17μg／kg，回收率为97．2％-102．3％。

The method for determination of Metanil Yellow dyes in silk fabrics using solid phase extraction- ultrafast liquid chromatography coupled with electrospray ionization tandem mass spectrometry （SPE UFLC-ESI-MS/MS） is established. The samples are extracted and purified by solid phase extraction （SPE） cartridge, UFLC separation is performed on an ACQUITY UPLCTM BEH C18 column utilizing a gradient elution program of acetonitrile（containing O. 1% formic acid） and water （containing 0.1% formic acid） as the mobile phase. Identification and quantification are carried out by UFLC-ESl MS/MS in negative mode and multiple reactions monitoring. Good linearity is observed in the range of 0.5-100.0 μg/L with correlation coefficients 0.999 5, limit of detection （LOD） for Metanil Yellow dyes is 0.17 μg/kg. The recovery ranges from 97.2% to 102.3%.