液相色谱-内置可控在线电解制氢-原子荧光光谱法测定鱼类水产品中汞形态OA

To align with the development trend of green analytical chemistry,this study adopted built-in pure-water electrolysis hydrogen generation technology,and utilizing an unattended mode es-tablished a novel analytical method for mercury speciation determination using liquid chromatogra-phy-atomic fluorescence spectrometry(LC-AFS).The experimental results revealed good linearity of the mercury species concentrations in the range of 0-100 μg/L,with correlation coefficients(r)ex-ceeding 0.999.The inorganic mercury,methylmercury,and ethylmercury detection limits were 0.005,0.004,and 0.004 mg/kg,respectively.The methylmercury determination sensitivity was significantly improved compared with that of traditional LC-AFS.The recoveries at different concen-tration levels ranged from 81.0%to 107%,and the relative standard deviations were less than 5%.The mercury speciation determination results for the certified reference materials,namely,tuna(ERM-CE464)and fish muscle(GBW10029),were both within the range of the certified standard values.Certain deep-sea fish have been shown to contain high levels of methylmercury,which em-phasizes the food safety concerns associated with methylmercury in carnivorous fish.Compared with the currently mainstream traditional LC-AFS method for mercury speciation determination,the pro-posed method significantly reduced the usage of hydrochloric acid,potassium borohydride,and po-tassium persulfate,and decreased the waste-liquid generation.Additionally,this technique em-ployed a unique concentric-structure semi-shielded rectangular tube,which effectively prevented flu-orescence quenching while substantially reducing the argon-gas consumption.Overall,the proposed method is highly sensitive and accurate and suitable for the analysis and determination of mercury spe-ciation in fish aquatic samples.Moreover,this method constitutes a low-cost and environmentally-friendly mercury speciation analysis technique.