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| 海藻中铝形态分析技术 |
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尚德荣1,2, 赵艳芳1,2, 张继红1, 宁劲松1,2, 翟毓秀1,2, 郭莹莹1,2, 丁海燕1,2, 盛晓风1,2
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1.中国水产科学研究院黄海水产研究所，青岛 266071;2.农业部水产品质量安全检测与评价重点实验室 国家水产品质量监督检验中心，青岛 266071
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| 摘要: |
| 建立了高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP-MS）分析海藻及其制品中三价铝的方法，用提取液0.040 mol/L 氢氧化锂 +0.006 mol/L吡啶-2，6-二羧酸+0.090 mol/L冰醋酸在70℃恒温水浴摇床中浸提2 h，阳离子交换色谱柱分离， ICP-MS检测。样品加标量在5.0 mg/kg和50.0 mg/kg时的平均回收率在90.8%以上，相对标准偏差均<4%（n=5）。本研究证明，该方法测定海藻及其制品中的三价铝较为准确、可靠，可为制定农业行业标准提供技术支撑。 |
| 关键词: 铝 形态 海藻 高效液相色谱 电感耦合等离子体质谱 |
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| 基金项目:2011农业部财政专项-藻类产品中重金属存在形态及检测方法研究、农业行业标准（2011516）和国家“十二五”支撑课题子课题（2011BAD13B06）和中央级科研院所基本科研业务费（20603022011015） |
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| Speciation analysis of aluminum in the seaweed |
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| Abstract: |
| The analysis of aluminium (Al) in the seaweed is usually according to GB/T 23374-2009 which is in fact the method for measuring total Al. However, most of the Al in the seaweed exists in organic forms which can not be absorbed by biological organism, and the toxic soluble ionic Al (Ⅲ) is very low. So it is urgent to establish a method for the Al speciation analysis in the seaweed. In the present research, the liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) was used to determine the Al (Ⅲ) in the seaweed. The samples were extracted by the eluent (0.040mol/L LiOH,0.006 mol/L PDCA and 0.090 mol/L CH3COOH) and shaken under 70 ℃ for 2 h, and then the extract solution was centrifuged and filtered. After separation by CS5A column, the Al (Ⅲ) was tested by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The concentration of standard Al solutiors (Ⅲ) were 5.0mg/kg and50.0mg/kg, and the average recoveries were all above 90.8%, and the relative standard deviations were all below 4% (n=5). This method was successfully used in the analysis of real samples and proved to be very accurate and reliable, which may provide important technical support for drawing up the agricultural professional standard. |
| Key words: Aluminum Speciation Seaweed High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry |