ASE-LC-MS/MS技术检测水产品中三类溴系阻燃剂

Three Kinds of Brominated Flame Retardants TBBPA, BDE209 and HBCDs in Aquatic Product by ASE-LC-MS/MS

建立了快速溶剂萃取-超快速液相色谱-串联质谱（ASE-LC-MS/MS）法测定水产品中四溴双酚A、十溴联苯醚和六溴环十二烷三类溴系阻燃剂含量的方法。样品经C18色谱柱分离,以水和甲醇为流动相,质谱多反应监测（MRM）模式检测,基质标准校正,外标法定量。四溴双酚A、十溴联苯醚和六溴环十二烷三类溴系阻燃剂定量限（S/N=10）为3.0μg/kg和5.0μg/kg,并在1.0~100μg/L范围内线性关系良好,相关系数r≥0.998 8。在3个加标水平下激素的加标回收率为83.6%~95.9%,相对标准偏差为4.88%~8.24%（n=6）。该方法具有优异的灵敏度与稳定性,满足对水产品中三类溴系阻燃剂分析检测及准确定量。

A new method was established for three kinds of brominated flame retardants TBBPA, BDE209 and HBCDs in aquatic product by the accelerated solovent extraction-ultra performance liquid chromatography-tandem mass spectrometry（ASE-LC-MS/MS） method. The target compounds were separated by a C18 column with methanol and water as the mobile phases in a multiple reaction monitoring（MRM） scan mode. External matrix standard solutions were used for the quantitative determination. As a result, the limits of quantification（S/N=10） were 3.0 μg/kg and 5.0 μg/kg, the calibration curves respectively showed a good linearity in the concentration range of 1.0~100 μg/L for TBBPA, BDE209 and HBCDs. The correlation coefficients were no less than 0.998 8. The average recoveries of the target compounds ranged from 83.6% to 95.9% with the relative standard deviations（RSDs） of 4.88%~8.24%（n=6）. The method was sensitive, stable and well suitable for the determination of three kinds of brominated flame retardants TBBPA, BDE209 and HBCDs in aquatic product.