气相色谱串联质谱(GC-MS／MS)法测定水产品中的9种合成麝香  

Determination of 9 synthetic musks in aquatic products by GC-MS/MS

作　　者：叶洪[1] 林永辉[2] 杨方[2] 刘正才[2] 卢声宇[2] 蓝锦昌[2] 

机构地区：[1]福建农林大学食品科学学院,福州350002 [2]福建省出入境检验检疫局技术中心,福州350001

出　　处：《分析试验室》2012年第11期45-49,共5页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科技项目(2012IK033)资助

摘　　要：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 reported in this work. The SMs were analyzed by GC-MS/MS under optimized conditions and quantitated by internal standard method with fluoranthene-D10 after the purification by florisil solid-phase extraction columns, following the hexane extraction for 30 minutes under uhrasonication. Results showed that the calibration curves of all 9 SMs were positively linear in the range of 0. 5 100μg/L （R2 〉0. 99） and the limits of quantification were form 0. 05 to 0. 10 μg/L. The average recoveries of SMs ranged from 76.42% to 113.25% with the relative standard deviations only from 2. 8% to 9.2%. In addition, galaxolide and tonalide were found for the first time in the shark, hairtail and nibea albiflora by the method here. Therefore, it is foreseen that this method was simple and accurate, capable of satisfying the determination of SMs analysis in aquatic products.

关 键 词：合成麝香 气相色谱质谱联用技术 水产品 佳乐麝香 吐纳麝香 

分 类 号：O657.63[理学—分析化学]