液相色谱-原子荧光光谱联用检测海产品中 不同形态锡的研究

Analysis of stannum species in marine products by high performance liquid chromatography-atom fluorescent spectrometry

中文关键词:  海产品  锡形态分析  液相色谱法  原子荧光

英文关键词:marine product  stannum speciation analysis  high performance liquid chromatography  atomic fluorescence spectrometry

中文摘要:

      目的: 建立液相色谱串联原子荧光光谱仪检测海产品中不同形态的锡的测定方法。方法: 选择合适的提取液和流动相V (乙腈) ：V ( 水 ) ：V ( 乙酸)：V ( 三乙胺 ) = 65：23：12：0.005来提高三甲基锡、一丁基锡、二丁基锡和三丁基锡的提取效率和分离度; 通过调整灯电流、负高压、载气和屏蔽气流量以及还原剂的浓度, 优化原子荧光检测条件, 使待测物的荧光强度达到最佳状态。结果: 本方法的三甲基锡、一丁基锡、二丁基锡和三丁基锡在10.0~ 100 μg/L 范围内有良好的线性, 方法的测定低限均为0.05 mg /kg; 实验表明方法对不同海产品的回收率在81.5% ~ 95.7%之间, 相对标准偏差在1.0% ~ 5.1%之间。结论: 该方法简便、准确, 所使用的设备价格低廉, 可用于海产品中4种锡形态的测定。

英文摘要:

      Objective To establish a method for determination of four different stannum species in marine products by high performance liquid chromatography-atom fluorescent spectrometry (HPLC-AFS). Methods The solution which contained 65% acetonitrile, 23% water, 12% acetic acid and 0.005% three triethylamine was used to increase the extraction efficiency of trimethytin (TMT), monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT), and to be the optimized mobile phase. The lamp current, negative high voltage, velocity of carrier gas, velocity of auxiliary gas, and concentrations of reducing agent were also optimized. Results The linear ranges for TMT, MBT, DBT and TBT were all from 10 to 100 μg/L. The detection limits of TMT, MBT, DBT and TBT were 0.05 mg/kg. The recoveries of the method were 81.5%~95.7% (n= 8), and the relative standard deviations were 1.0%~5.1%. Conclusion This method is simple and convenient, and can be used to analyze the four stannum species in marine products.