建立了超高效液相色谱-串联质谱法(uHPlC-MS/MS)同时测定纺织品中2,4-二氯苯酚(2,4-dCP)、2,4,6-三氯苯酚(2,4,6-TrICP)、2,3,4,6-四氯苯酚(2,3,4,6-TECP)、五氯苯酚(PCP)、辛基苯酚(OP)、壬基苯酚(nP)、邻苯基苯酚(OPP)、双酚A(bPA)、四溴双酚A(TbbPA)9种酚类化合物的方法.样品在密闭萃取瓶中于60℃用甲醇超声萃取1H后,待测酚类化合物用zOrbAX Xdb-C18色谱柱分离,电喷雾负离子模式(ESI-)电离、多重反应监测(MrM)模式测定,外标法定量.方法优化了超声萃取条件、色谱分离条件及质谱碎裂电压、碰撞能量等质谱测定条件.在优化实验条件下,方法相对标准偏差(rSd)为5.1%(PCP)~9.7%(2,3,4,6-TECP)(n=7),对9种酚类化合物3个浓度水平的加标回收率在82%(2,3,4,6-TECP)~120%(OP)之间,方法定量限(lOQS)在0.03Mg/kg(PCP)~1.5Mg/kg(TbbPA)之间,线性范围为0.05~10Mg/l.该方法具有样品处理步骤简捷、分析速度快、选择性好、灵敏度高等特点,能同时完成纺织品中9种酚类化合物的定性与定量分析.A method was developed for simultaneous quantification of 2,4-dichlorophenol(2,4-DCP),2,4,6-trichlorophenol(2,4,6-TriCP),2,3,4,6-tetrachlorophenol(2,3,4,6-TeCP),pentachlorophenol(PCP),4-tert-octylphenol(OP),nonylphenol(NP),o-phenyl phenol(OPP),bisphenol A(BPA),and tetrabromobisphenol A(TBBPA)in textiles with ultra high performance liquid chromatography-tandem electrospray ionization mass spectrometry(UHPLC-MS/MS).Textile samples were extracted in a closed bottle at 60℃with methanol with ultrasonic extraction for 1h.Target compounds were separated by Zorbax XDB-C18column and gradient eluted with methanol and water containing 0.075% ammonium hydroxide,and then determined with negative electrospray ionization mass spectrometry at multiple reactions monitoring mode(MRM).Quantitative analysis was performed with external standard calibration.Operating parameters,such as ultrasonic extraction condition,UHPLC separation condition,concentration of ammonium hydroxide in mobile phase,fragment voltages,and collision energies,were optimized.Relative standard deviation(RSDs)for developed method were in the range of 5.1%(PCP)and 9.7%(2,3,4,6-TeCP)(n=7).Recoveries in sample matrix ranged from 82%(2,3,4,6-TeCP)to 120%(OP).The limit of quantification(LOQs)was from 0.03mg/kg(PCP)to 1.5mg/kg(TBBPA).The proposed method was simple,rapid,accurate,sensitive and suitable for simultaneous determination of nine phenol compounds in a variety of textiles.福建省泉州市丰泽区科技项目(2012FZ17); 远东技术服务有限公司委托项
