Key Laboratory of Green Chemistry & Technology of MOE, College of Chemistry, Sichuan University , Chengdu, Sichuan 610064, China.
Analytical & Testing Center, Sichuan University , Chengdu, Sichuan 610064, China.
Anal Chem. 2017 Feb 7;89(3):2093-2100. doi: 10.1021/acs.analchem.6b04753. Epub 2017 Jan 24.
Sensitive quantification of mercury distribution in fish is challenging because of insufficient sensitivities of conventional analytical methods, the limited mass of organs (tens of micrograms to several milligrams), and dilution of analyte concentration from sample digestion. In this work, a simple and robust approach coupling multiwall carbon nanotubes assisted matrix solid-phase dispersion (MWCNTs-MSPD) to single-drop solution electrode glow discharge-induced cold vapor generation (SD-SEGD-CVG) was developed for the sensitive determination of mercury in limited amount of sample. Mercury species contained in a limited amount of sample can be efficiently extracted into a 100 μL of eluent by MWCNTs-MSPD, which are conveniently converted to Hg by SD-SEGD-CVG and further transported to atomic fluorescence spectrometry for their determination. Therefore, analyte dilution resulted from sample preparation is avoided and sensitivity is significantly improved. On the basis of consumption of 1 mg of sample, a limit of detection of 0.01 μg L (0.2 pg) was obtained with relative standard deviations (RSDs) of 5.2% and 4.6% for 2 and 20 μg L, respectively. The accuracy of the proposed method was validated by analysis of three Certified Reference Materials with satisfying results. To confirm that SD-SEGD-CVG-AFS coupling to MWCNTs-MSPD is a promising method to quantify mercury distribution in fish, this method was successfully applied for the sensitive determination of mercury in seven organs of common carps (muscle, gill, intestine, liver, gallbladder, brain, and eye) after dietary of mercury species. The proposed method provides advantages of minimum sample dilution, low blank, high sample introduction efficiency, high sensitivity, and minimum toxic chemicals and sample consumption.
由于传统分析方法的灵敏度不足、器官质量有限(数十微克到数毫克)以及样品消化过程中分析物浓度的稀释,因此对鱼类中汞分布的敏感定量具有挑战性。在这项工作中,开发了一种简单而强大的方法,将多壁碳纳米管辅助基质固相分散(MWCNTs-MSPD)与单滴溶液电极辉光放电诱导冷蒸气发生(SD-SEGD-CVG)相结合,用于对有限量样品中的汞进行灵敏测定。通过 MWCNTs-MSPD 可以将有限量样品中含有的汞形态有效地提取到 100μL 的洗脱液中,然后通过 SD-SEGD-CVG 将其方便地转化为 Hg,并进一步运送到原子荧光光谱仪进行测定。因此,避免了样品制备带来的分析物稀释,灵敏度得到显著提高。在消耗 1 毫克样品的基础上,该方法的检出限为 0.01μg L(0.2pg),对于 2 和 20μg L 的相对标准偏差(RSD)分别为 5.2%和 4.6%。通过对三种认证参考物质的分析验证了该方法的准确性,结果令人满意。为了确认 SD-SEGD-CVG-AFS 与 MWCNTs-MSPD 的结合是定量鱼类中汞分布的一种很有前途的方法,该方法成功地应用于七种鲤鱼器官(肌肉、鳃、肠、肝、胆囊、脑和眼)中汞形态的饮食后,对汞的灵敏测定。该方法具有最小样品稀释、低空白、高样品引入效率、高灵敏度以及最小毒性化学物质和样品消耗的优点。