Analytical Sciences

Direct Determination of Lead in Foods by Solid Sampling Electrothermal Vaporization Atomic Fluorescence Spectrometry

Derong SHANG,* Yanfang ZHAO,* Yuxiu ZHAI,* Jinsong NING,* Delin DUAN,** and Yongdong ZHOU***

*Yellow Sea Fishery Research Institute Chinese Academy of Fishery Sciences, Nanjing Road 106, Qingdao 266071, China
**Institute of Oceanology, Chinese Academy of Sciences, Nanhai Road 7, Qingdao 266071, China
***Yancheng Hairui Food Co. Ltd., Dafeng 224005, China

A solid sampling method for the determination of lead in foods (including grains, vegetables and seafoods) using electrothermal vaporization atomic fluorescence spectrometry was established. The method introduced samples using electrothermal vaporization by quartz furnace and used on-line ashing and vaporization to remove matrix interferences for the specific trap of lead. It was proven by the certified reference material (CRM) and the recovery rate of the standards that the electrothermal vaporization was stable and there was no effect for sampling difference. The best operating program and parameters for the new method included ashing (850°C, 160 s), vaporization and trap (1050°C, 80 s; 800°C, 10 s), release (800°C, 10 s), and mixed Ar + H₂ (85:15%, v/v) as carrier gas with flow rate of 500 mL/min. The relative standard deviations of repeated Pb measurements in CRMs were all below 5.0%, and the recovery rate ranged from 90.0 – 110.0%. The limit of detection (LOD) for the new method was 3.0 pg and the limit of quantification (LOQ) was 10.0 pg. The total time of analysis was less than 6 min. No significant differences existed between the results measured by the new method and microwave ICP-MS.

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