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目的采用高压液相色谱-氢化物发生-原子荧光光谱联用技术(HPLC-HG-AFS)对水产品中硒的赋存形态检测进行研究。方法通过实验优化流动相、提取剂、提取时间及其仪器条件,建立HPLC-HG-AFS联用技术检测水产品中硒形态的分析方法。用去离子水在70℃水浴下超声提取1 h,流动相为pH 6.0的40mmol/L(NH4)2HPO4溶液,阴离子交换柱分离,HG-AFS检测。结果样品加标量在0.10、1.00 mg/kg时的回收率均在86.6%以上,相对标准偏差均小于5%。结论本研究证明使用该方法测定水产品中的硒形态较为准确、可靠,为科学评价水产品质量、进一步细化富硒水产品的判定标准和鉴别其真伪提供技术手段,为科学有效地开展其风险评估提供技术支撑和数据支持。
OBJECTIVE To study the speciation of selenium in aquatic products by HPLC-HG-AFS with high pressure liquid chromatography-hydride generation-atomic fluorescence spectrometry. Methods The mobile phase, extractant, extraction time and instrument conditions were optimized through experiments. The analytical method of HPLC-HG-AFS was established for the determination of selenium in aquatic products. The samples were extracted with deionized water for 1 h under 70 ℃ water bath. The mobile phase consisted of 40 mmol / L (NH4) 2HPO4 solution with pH 6.0, separated by anion exchange column and detected by HG-AFS. Results The recoveries of the sample with the standard addition of 0.10 and 1.00 mg / kg were above 86.6% with relative standard deviations less than 5%. CONCLUSIONS This study demonstrates that the method for the determination of selenium in aquatic products is more accurate and reliable. It is a scientific and effective method to scientifically evaluate the quality of aquatic products, further refine the determination criteria of selenium-enriched aquatic products and identify their authenticity. Its risk assessment provides technical support and data support.