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[目的]采用气相色谱-质谱串联技术,建立测定斑马鱼(Zebrafish,Danio rerio)和稀有鮈鲫(Rare gudgeon,Gobiocypris rarus)体内二甲苯麝香的分析方法。[方法]鱼样通过快速溶剂萃取和凝胶渗透色谱净化后,采用选择离子方式进行检测,外标法定量。[结果]该方法的检测限为4μg/L,线性范围为10～400μg/L。该方法进行的20μg/L和100μg/L的2个加标浓度的测试结果显示,斑马鱼加标的平均回收率分别为108.0%和97.4%,相对标准偏差分别为4.9%和9.3%;稀有鮈鲫加标的平均回收率分别为104.0%和112.0%,相对标准偏差分别为10.0%和10.0%;均符合回收率80%～120%和相对标准偏差<15%的要求。[结论]该方法灵敏度高,线性范围宽,杂质干扰小。采用该法对我国特有水产品稀有鮈鲫体内二甲苯麝香进行了分析检测,结果表明该法适用。
[Objective] To establish an analytical method for the determination of musk xylene in zebrafish (Zebrafish, Danio rerio) and Rare gudgeon (Gobiocypris rarus) using gas chromatography-mass spectrometry tandem technology. [Method] After the samples were purified by rapid solvent extraction and gel permeation chromatography, the samples were detected by selective ion method and quantified by external standard method. [Result] The detection limit of this method was 4μg / L and the linear range was 10 ~ 400μg / L. The results of two spiked concentrations of 20μg / L and 100μg / L by this method showed that the average recoveries of zebrafish spikes were 108.0% and 97.4%, respectively, and the relative standard deviations were 4.9% and 9.3%, respectively. The average recoveries of crucian carp were 104.0% and 112.0%, respectively. The relative standard deviations were 10.0% and 10.0%, respectively. All of them met the requirements of recovery of 80% -120% and relative standard deviation of <15%. [Conclusion] The method has high sensitivity, wide linear range and small impurity interference. The method was used to analyze the musk of xylene in the rare crucian carp (Carassius auratus gibelio), an endemic aquatic product, in China. The results show that this method is suitable.