分散固相萃取-气相色谱-质谱联用法测定水产品中的痕量酮麝香

Determination of musk ketone in aquatic products by gas chromatography-mass spectrometrywith dispersive solid phase extraction

建立了水产品中痕量酮麝香测定的分散固相萃取－气相色谱－质谱联用法（GC—MS）．目标化合物经1％乙酸－乙腈高速匀浆提取，以Ｎ－丙基乙二胺（PSA）、C18和石墨化碳（GCB）混合物为分散剂对其进行净化，采用GC—MS在选择离子检测式下测定，外标法定量，幷应用正交试验对前处理条件进行优化．以及对酮麝香的裂解机制进行探涛。在优化条件下，方法载1～50μg／L范围内线性关系良好，相关系数不低于0．999，检出限（s／N=3）为0．30μg／kg对于明虾和罗非鱼空白样品，在1．0、2．0、10．0μg／kg3个水平下的加标回收率为91．8％～110．6％，相对标准偏差（RSD）为2．6％～8．4％。该方法操作简便、快速、准确，可用于水产品中痕量酮麝香的日常检验。

A dispersive solid phase extraction coupled with gas chromatography-mass spec- trometry （GC-MS） method was established for the determination of trace amounts of musk ketone in aquatic products. The target analyte in the samples was extracted with acetonitrile containing 1% acetic acid, cleaned-up with the mixture of N-propyl-ethylenediamine （PSA）, C18 and graphitized carbon （GCB）, and analyzed by GC-MS under selected ion monitoring （SIM） mode and quantified by the external standard method. The orthogonal experiment was carried out to optimize the pre-treatment conditions. Under the optimal conditions, good linear relationship was obtained in the range of I -50 μg/L for musk ketone with correlation coeffi- cient not less than 0. 999, and the limits of detection （S/N = 3 ） was 0.30 μg/kg. The recover- ies of musk ketone in the prawn and tilapia blank samples at three spiked levels of I. 0, 2.0 and 10.0 μg/kg ranged from 91.8% to 110.6% with RSDs in the range of 2.6% - 8.4%. The method is simple, rapid and accurate, and can be used for the routine analysis of musk ketone in aquat- ic products.