【摘要】 目的：采用超声萃取结合¹³C₁₂稳定同位素内标-气相色谱-串联质谱（GC-MS/MS）法，对广东部分市售淡水鱼中6种羟基多溴联苯醚进行测定与分析。方法：样品的提取方式采用超声萃取，添加6-OH-[¹³C₁₂]-BDE-47内标后，利用固相萃取柱净化，N-（叔丁基二甲硅烷基）-N-甲基三氟乙酰胺（MTBSTFA）衍生，选择电子轰击源（EI）和动态多反应监测模式（dMRM）气相色谱-串联质谱法进行测定。结果:广东部分市售淡水鱼中6种羟基多溴联苯醚在0.5ng/mL～100ng/mL范围内均呈良好线性关系，相关系数r>0.990。仪器检出限为0.10ng/g～0.25ng/g。加标回收率为74.6%～93.8%，相对标准偏差3.26%～10.8%。结论:该方法灵敏度高，特异性好，操作简便，准确度和精密度高，可满足淡水鱼类中6种羟基多溴联苯醚的检测要求。更多还原

【Abstract】 This study employed ultrasound-assisted extraction coupled with ¹³C₁₂-labeled internal standard gas chromatography-tandem mass spectrometry（GC-MS/MS） for the determination of six hydroxylated polybrominated diphenyl ethers（OH-PBDEs） in selected commercially available freshwater fish from Guangdong Province. Ultrasonic extraction was used for sample extraction. After adding the internal standard of 6-OH-[¹³C₁₂]-BDE-47, solid-phase extraction（SPE） with acidic silica gel was used for purification. Derivatization treatment was carried out with the silylation reagent（MTBSTFA）. The electron impact source（EI） and the dynamic multiple reaction monitoring mode（d MRM） gas chromatography-tandem mass spectrometry were selected for determination. The six hydroxylated polybrominated diphenyl ethers（OH-PBDEs） in commercially available freshwater fish from parts of Guangdong showed good linearity within the range of 0.5 to 100ng/m L, with correlation coeficients（r） greater than 0.990. The detection limits of the instrument were between 0.10ng/g and 0.25ng/g. The average recoveries were between 74.6% and 93.8%, with relative standard deviations（RSDs） ranging from 3.26% to 10.8%. This method demonstrates high sensitivity, excellent specificity, a straightforward procedure, and superior accuracy/precision.更多还原