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

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在选择离子监测模式下测定,外标法定量,并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讨。在优化条件下,方法在1～50 μg/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0.30 μg/kg。对于明虾和罗非鱼空白样品,在1.0、2.0、10.0 μg/kg 3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。

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

A dispersive solid phase extraction coupled with gas chromatography-mass spectrometry (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 1-50 μg/L for musk ketone with correlation coefficient not less than 0.999, and the limits of detection (S/N=3) was 0.30 μg/kg. The recoveries of musk ketone in the prawn and tilapia blank samples at three spiked levels of 1.0, 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 aquatic products.