多重吸附同步净化-气相色谱-质谱联用法测定水产品中痕量的二甲苯麝香和酮麝香

为了考察水产品中二甲苯麝香和酮麝香的残留量，建立了水产品中痕量二甲苯麝香和酮麝香测定的多重吸附同步净化（MASP）-气相色谱-质谱联用法（GC-MS）。以乙腈高速匀浆提取样品，应用MASP方法对样品同时进行提取、盐析和净化，并采用GC-MS在选择离子监测（SIM）模式下测定水产品中的痕量二甲苯麝香和酮麝香，以基质匹配标准溶液外标法定量。选用DB-5 MS石英毛细管柱（30 m×0.25 mm×0.25 μm），采用电子轰击电离源，二甲苯麝香的选择监测离子为m/z 282、297、265，酮麝香为m/z 279、294、191。结果表明：在优化条件下，二甲苯麝香和酮麝香在1~100 μg/kg范围内线性良好，相关系数不低于0.999，检出限（S/N=3）为0.30 μg/kg。明虾、花蛤和鳗鱼空白样品中1.0、2.0、10.0 μg/kg 3个添加水平下二甲苯麝香和酮麝香的加标回收率为79%~104%，相对标准偏差（RSD）为1.6%~13.3%。本方法具有操作简便、快速、准确的特点，可用于水产品中痕量二甲苯麝香和酮麝香的日常检测。

Determination of trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

In order to investigate the residues of musk xylene and musk ketone in aquatic products, a method was established for the determination of the trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification (MASP)-gas chromatography-mass spectrometry (GC-MS). After extracted with acetonitrile, the samples were pretreated using MASP method including extraction, salting-out and purification processes, analyzed with GC-MS in the selected ion monitoring (SIM) mode, and then quantified by matrix-matched standard solution in external standard method. The analysis was carried out with a capillary column (DB-5 MS, 30 m×0.25 mm×0.25 μm) under electron ionization conditions. The quantification was performed using monitoring ions of m/z 282, 297, 265 for musk xylene and m/z 279, 294, 191 for musk ketone. The results showed good linearity in the range of 1-100 μg/kg for musk xylene and musk ketone with the correlation coefficients not less than 0.999, and the limits of detection (S/N=3) of 0.30 μg/kg. The average recoveries of musk xylene and musk ketone spiked in prawn, clam and sea eel blank samples at three spiked levels of 1.0, 2.0 and 10.0 μg/kg ranged from 79% to 104% and the RSDs were in the range of 1.6%-13.3%. The method is simple, rapid and accurate, and can be used for the routine analysis of musk xylene and musk ketone in aquatic products.