采用液相色谱-串联质谱法对鱼肉和虾肉中三苯甲烷类与噻嗪类染料及其代谢物进行测定.样品经对甲苯磺酸-乙酸铵-乙腈溶液提取,正己烷脱脂,二氯甲烷萃取,MCAX固相萃取净化后,以Waters BEH C18色谱柱为分离柱,以0.15%甲酸溶液(含5 mmol·L-1乙酸铵溶液)-乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源及多反应监测模式进行测定.各化合物的质量浓度在20.0 μg·L-1以内呈线性,方法的测定下限(10S/N)均为0.5 μg·kg-1.对空白样品进行加标回收试验,回收率在62.6%~108%之间,测定值的相对标准偏差(n=6)在2.0%~14%之间.方法用于鱼肉和虾肉样品的检测,结果与国家标准方法的测定值一致.

A method of LC-MS/MS was applied to determine triphenylmethane,thiazide and their metabolites in fish and shrimp samples. The sample was extracted with a mixture of p-toluenesulfonic acid,ammonium acetate and acetonitrile,defatted with hexane,extracted with dichloromethane,and then purified with MCAX solid phase extraction column. Waters BEH C18 column was used as stationary phase and the mixture of 0.15% formic acid solution (with 5 mmol·L-1 ammonium acetate) and acetonitrile was used as mobile phase for gradient elution. ESI+ and MRM were adopted in MS/MS. The linearity ranges of the compounds were found within 20.0 μg·L-1,with limits of quantification (10S/N) of 0.5 μg·kg-1. Recovery rate measured by standard addition method was in the range of 62.6%-108% with RSD′s (n=6) in the range of 2.0%-14%. The method was used to analyze of fish and shrimp samples,giving results consistent with those obtained by the standard method.