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建立了气相色谱串联质谱技术(GC-MS/MS)测定水产品中9种合成麝香(SMs)的方法。对方法前处理条件和质谱条件进行优化,确定样品采用正己烷超声波振荡提取30 min,硅胶固相萃取柱净化,气相色谱串联质谱测定,内标法定量(内标物质为荧蒽-D10)。9种合成麝香的线性范围为0.5～100μg/L,检出限为0.05～0.10μg/L,相关系数均大于0.99。添加回收实验中,9种合成麝香的平均回收率为76.4%～113.3%,标准偏差为2.8%～9.2%。利用本方法,在鲨鱼、带鱼和黄姑鱼样品中检测出了佳乐麝香和吐纳麝香。
A method for the determination of 9 synthetic musks (SMs) in aquatic products by gas chromatography-tandem mass spectrometry (GC-MS / MS) was established. The pretreatment conditions and mass spectrometry conditions were optimized. The samples were extracted with n-hexane and sonicated for 30 min. The samples were purified by silica gel column chromatography and determined by gas chromatography-tandem mass spectrometry. The internal standard method was used for quantitative determination (fluoranthene-D10). The linear range of the 9 synthetic musk was 0.5 ~ 100μg / L, the detection limit was 0.05 ~ 0.10μg / L, the correlation coefficient was greater than 0.99. In the recovery experiments, the average recoveries of nine synthetic musk species ranged from 76.4% to 113.3% with standard deviations from 2.8% to 9.2%. Using this method, musk and venom musk were detected in shark, octopus and yellow croaker samples.