纺织品和皮革中10种酚类化合物的同时测定——高效液相色谱-串联质谱法

Simultaneous Determination of Ten Phenols in Textiles and Leather Products by High Performance Liquid Chromatography-tandem Mass Spectrometry

建立了高效液相色谱一串联质谱（HPLC—MS／MS）联用技术同时测定纺织品和皮革中10种酚类化合物的方法。样品经甲醇超声提取、浓缩后，经OasisHLB固相萃取柱净化，采用EclipseExtend—C18色谱柱（2．1mm×100mm，3．5μm），乙腈和0．01mol／L甲酸铵水溶液（pH=6．3）为流动相梯度洗脱，电喷雾离子源电离，负离子多反应监测模式进行定性和定量分析。10种酚类化合物在0．08—5mg／L浓度范围内与峰面积呈良好的线性关系，相关系数为0．9931—0．9993；以不低于3倍的信噪比计算10种酚类化合物的检出限（LOD）为0．0001—0．0034mg／kg；定量限（LOQ，S／N≥10）为0．0005～0．0113mg／kg。棉、麻、毛、皮革4种基质在3个不同加标水平的回收率为77％～108％，相对标准偏差（RSDs）为1．7％～10．8％。该方法能同时完成10种酚类化合物的确证和分析，适用于纺织品和皮革中酚类化合物残留的检测分析。’

A method has been developed for the simuhaneous extraction and determination of ten phenols in textiles and leather products by high performance liquid chromatography coupled with electrospray ionization tandem mass spectrome- try （HPLC-ESI-MS/MS）. The samples were extracted with methanol under ultrasonic assistance and purified by solid phase extraction （SPE） with Oasis HLB SPE column. The separation of ten phenols was performed on an Eclipse Extend- C18 column （2.1 mm×100mm,3.5μm ） using acetonitrile -water （containing 0.01 mol/L ammonium formate, pH 6.3）as the mobile phase. Identification and quantification were achieved by HPLC-ESI-MS/MS in negative mode and multiple reactions monitoring. The result indicated that the calibration curves of ten phenols showed good linear relationships be- tween peak area and concentration in the range of 0.08-5 mg/L, with correlation coefficients of 0.9931-0.9993. The limits of detection （ LODs, S/N 〉13） of ten phenols were in the range of 0.0001 -0.0034 mg/kg, and the limits of quantitation （LOQs, S/N ≥ 10） were 0.0005 -0.0113 mg/kg. The average recoveries of ten phenols from 4 typical textile and leather ma- trices including cotton, wool, ramie and leather, at three spiked concentration levels were in the range of 77 %-108 % with relative standard deviations （RSDs） of 1.7%-10.8%. The results indicated that the method was rapid, selective, sensi- tive and stable enough to detect the 10 phenols in textile and leather samples.