超高效液相色谱-串联质谱法快速测定鱼肉样品中的三氯生和三氯卡班

Rapid determination of triclosan and triclocarban in fish by ultra-performance liquid chromatography tandem mass spectrometry

目的建立鱼肉样品中三氯生和三氯卡班的Qu ECh ERS-超高效液相色谱-串联质谱快速测定方法。方法鱼肉样品经乙腈提取,十八烷基硅烷键合硅胶(C_(18))净化粉净化,甲醇和水为流动相梯度洗脱,采用电喷雾负离子模式电离,超高效液相色谱-串联质谱仪多反应监测模式,以保留时间和目标物的二级质谱特征碎片离子定性,内标法定量。结果三氯生和三氯卡班在1.0 ng/ml~200.0 ng/ml,回归方程呈良好的线性关系,相关系数>0.99。检出限和定量限分别为0.06μg/kg~0.37μg/kg和0.18μg/kg~1.23μg/kg,回收率为105.4%~115.4%,相对标准偏差为1.60%~5.75%。结论通过优化液相、质谱和前处理条件,建立了超高效液相色谱-串联质谱法测定鱼肉中三氯生和三氯卡班的方法,该方法操作简单快捷,灵敏度高,选择性好。

Objective To establish a rapid method of Qu ECh ERS-ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)for the determination of triclosan and triclocarban in fish.Methods The fish samples were extracted with acetonitrile and purified with actadecyl silane bonded silica gel(C;)purification powder.The target compounds were quantified by UPLC-MS/MS with methanol-water as the mobile phase in gradient elution.Electrospray ionization mass spectrometry was carried out in negative ion mode with multiple reaction monitoring(MRM)mode.Qualitative analysis was done by both retention time and secondary mass fragment ions,and quantitative analysis was done by internal standard curve.Results The linear correlations of triclosan and triclocarban were good in 1.0 ng/ml-200.0 ng/ml,with the correlation coefficients greater than 0.99.The limits of detection and limits of quantification were 0.06μg/kg-0.37μg/kg and0.18μg/kg-1.23μg/kg,respectively.Satisfactory recoveries(105.4%-115.4%)and RSDs(1.60%-5.75%)were achieved.Conclusion The UPLC-MS/MS method was established by optimizing the liquid chromatography,the mass spectrometry and the pretreatment conditions.The validated method was simple,rapid,accurate and sensitive for the measurement of triclosan and triclocarban in fish.