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  

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

作　　者：丁立平 蔡春平[2] 林永辉[2] 吴文凡 方祥 

机构地区：[1]福清出入境检验检疫局技术中心,福建福清350300 [2]福建出入境检验检疫局技术中心,福建福州350001

出　　处：《色谱》2014年第3期309-313,共5页Chinese Journal of Chromatography

基　　金：国家质检总局资助项目(2012IK033);福建出入境检验检疫局研究项目(FK2012-16)

摘　　要：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×0.25μm），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1～100μg / kg 范围内线性良好，相关系数不低于0.999，检出限（S / N =3）为0.30μg / kg。明虾、花蛤和鳗鱼空白样品中1.0、2.0、10.0μg / 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。In order to investigate the residues of musk xylene and musk ketone in aquatic prod-ucts,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 chro-matography-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＆#215;0. 25 mm＆#215;0. 25 μm）under electron ionization condi-tions. 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＆amp;nbsp;musk xylene and musk ketone in aquatic products.

关 键 词：多重吸附同步净化 气相色谱-质谱 二甲苯麝香 酮麝香 水产品 multiple adsorption synchronous purification( MASP) gas chromatography-mass spectrometry(GC-MS) 

分 类 号：O658[理学—分析化学]