该文建立了微波萃取结合高效液相色谱-电感耦合等离子体质谱(high performance liquid chromatography-inductively coupled plasma-mass spectrometry,HPLC-ICP-MS)联用技术测定干制食用菌中甲基汞(metHg)、乙基汞(etHg)、苯基汞(phHg)及无机汞(Hg2+)的方法。对不同提取方法的效果进行比较,并对流动相组分进行优化,结果表明,在12 min内可以实现无机汞、甲基汞、乙基汞、苯基汞的分离。线性关系良好(r＞0.999 0),相对标准偏差(relative standard deviation,RSD)≤10.0%,方法定量限分别为0.009、0.024、0.018和0.024 mg/kg。以牛肝菌、松茸、羊肚菌3种基质样品进行加标回收实验,回收率为77.5%～117.5%,采用2种标准物质GBW10029和Tort-3验证了方法的准确性,满足分析要求。此方法前处理简单、样品提取效率高,分离效果好,准确度高,适用于干制食用菌中汞形态的定量分析要求,为食用菌中汞形态分析提供了一种方法依据,推动食用菌甲基汞限量值的制定提供基础数据。
A method for the determination of methyl mercury (metHg),ethyl mercury (etHg),phenyl mercury (phHg) and inorganic mercury (Hg2+) in dried edible fungi by microwave extraction coupled with HPLC-ICP-MS was established.Microwave-acid extraction was selected as the sample pretreatment method by comparing the effects of different extraction methods.And the components of mobile phase used in the experiment were optimized,the separation of metHg,etHg,phHg and Hg2+ could be achieved within 12 min.Moreover,the linear regression equation was good(r>0.999 0),RSD≤10.0% and the limits of quantitation (LOQ) were 0.009,0.024,0.018 and 0.024 mg/kg,respectively.Furthermore,the recovery rates of boletus,Tricholoma matsutake and morchella esculenta were 77.5%-117.5%.The accuracy of the method was verified by two reference materials GBW10029 and Tort-3.Above all,the method is simple,effective,accurate,and suitable for the quantitative analysis of mercury in dried edible fungi.It provides a method basis for mercury speciation analysis in edible fungi and basic data for the determination of methylmercury limit value in edible fungi.
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