高压液相色谱-氢化物发生-原子荧光光谱(HPLC-HG-AFS)联用技术检测水产品中硒的赋存形态

Selenium speciation analysis in aquatic products by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry

中文关键词:  高压液相色谱  氢化物发生原子荧光光谱  水产品  硒形态

英文关键词:high performance liquid chromatography  hydride generation atomic fluorescence spectrometry  aquatic products  selenium speciation

中文摘要:

      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40 mmol/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。

英文摘要:

      Objective The determination of selenium speciation in aquatic products by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry (HPLC-HG-AFS) was analyzed in this study. Methods The mobile phases, extraction reagents, extraction time and instrumental conditions were optimized and then selenium speciation in aquatic products was analyzed by HPLC-HG-AFS. Samples were extracted at 70 ℃ for 1 h by ultrasonic extraction and the flow phase was 40 mmol/L (NH4)2HPO4 (pH6.0). The different selenium speciation was separated with anion exchange column and detected by HG-AFS. Results The average recoveries of 0.10 mg/kg and 1.00 mg/kg in samples were all above 86.6% and the relative stan-dard deviations were all below 5% with a high accuracy. Conclusion The established method was accurate and reliable for selenium speciation analysis. It could provide technological support for scientific evaluation of the aquatic product quality, as well as the authenticity of the selenium enriched aquatic products. At the same time, the method also could provide important information for risk assessment of the aquatic products.