摘要:
本文建立了液相色谱-原子荧光法测定水产及其制品中汞形态的检测方法,并对实验所用的流动相种类,流速,pH,进样体积,还原剂及载流(HCl)浓度进行优化,在14 min内可以实现无机汞(Hg2+)、甲基汞(MeHg)、乙基汞(EtHg)的分离。三种形态的汞均可以呈现良好的线性关系(r>0.9990),相对标准偏差(RSD)≤ 5.0%,以5、20、100 ng/mL这三个添加量在不同的样品基质中添加混合标准溶液进行加标回收实验,得到三种汞形态的回收率分别为80.1%~95.8%,92.1%~105%,80.3%~97.6%,实验测定检出限分别为0.021、0.014、0.018 mg/kg。用本方法检测鱼肉组织标准物质BCR463和ERM-CE464,测定值与标准值均吻合,进一步验证了本方法的准确性和可靠性。该方法前处理简单,提取效率较高,适用于实际水产及其制品中汞形态的分析测定。
Abstract:
A confirmative method was developed with liquid chromatography-atomic fluorescence spectrometry(LC-AFS)to detect mercury species in aquatic animals and their products,and the type of flow phase,velocity,pH,injection volume,the concentration of reducing agent and load current(HCl)were optimized. Three mercury species,inorganic mercury(Hg2+),methyl mercury(MeHg),ethyl mercury(EtHg)was completely separated in 14 minutes. Experimental results showed that,three species of mercury were in good linearity(r>0.9990),and relative standard deviations(RSD)were less than 5.0%. Adding the mixture standard solution to the different samples with the addition of 5 ng/mL,20 ng/mL,100 ng/mL,respectively,to conduct the standard recovery test,The recoveries of Hg2+,MeHg,EtHg were 80.1%~95.8%,92.1%~105%,80.3%~97.6%,respectively,and the detection limit was 0.017,0.112,0.142 mg/kg,respectively. The fish tissue standard substance BCR463 and ERM-CE464 were measured by using this method,and the measured value was consistent with the standard value,which further verifies the accuracy and reliability of this method. Moreover,this method has simple pretreatmentand high extraction efficiency,so it is applicable to the detection of mercury species in aquatic products.
百度学术
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