斑马鱼和稀有鮈鲫体内二甲苯麝香的分析方法研究
Analytical Methodology for Musk Xylene in Zebrafish and Rare Gudgeon
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摘要:
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。 Abstract:Objective To identify and quantify musk xylene (MX) bioaccumulated in zebrafish (Danio rerio) and rare gudgeon (Gobiocypris rarus) by gas chromatography-mass spectrometry (GC-MS). Methods The pretreatment of fish samples in cluded accelerated solvent extraction (ASE) followed by gel permeation chromatography (GPC). The eluate was determined by GC-MS after concentrated. MX standard solution was used as external standard. Results The detection limit of this method was 4 μg/L; the range of linearity was between 10 μg/L and 400 μg/L, presenting a good linear relationship. Using this method, the recovery rates of 20 μg/L and 100 μg/L standard MX solution added to the zebrafish samples were 108.0% and 97.4% respectively; the relative standard deviations were 4.9% and 9.3% respectively. The recovery rates of 20μg/L and 100μg/L standard MX solution added to the rare gudgeon samples were 104.0% and 112.0% respectively; the relative standard deviations were 10.0% and 10.0% respectively. Both results met the requirements of recovery rate (80%-120%) and relative deviation (<15%). Conclusion This method is featured by high sensitivity, wide linear range, and low impurity interference. The results show that the method is suitable for detection of MX in rare gudgeon.
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