高效液相色谱-电感耦合等离子体质谱法测定海洋贝类中的无机镉离子

Determination of inorganic cadmium ion in marine shellfish by high performance liquid chromatography-inductively coupled plasma mass spectrometry

中文关键词:  无机镉离子  高效液相色谱法  电感耦合等离子体质谱法  海洋贝类

英文关键词:inorganic cadmium ion  high performance liquid chromatography  inductively coupled plasma mass spectrometry  marine shellfish

中文摘要:

      目的 建立高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma mass spectrometry, HPLC-ICP-MS)检测海洋贝类中无机镉离子的分析方法。方法 取一定量样品加入10 mmol/L Tris-HCl(其中加入0.1 mol/L NaCl溶液)提取液, 超声萃取2 h, 离心过滤后至进样瓶中上机测定。流动相为30 mmol/L草酸水溶液和55 mmol/L氢氧化钾水溶液, 经CS5A阳离子交换色谱柱及CG5A保护柱对镉离子进行分离, 电感耦合等离子体质谱仪测定。结果 该方法线性关系良好, 相关系数r=0.998, 且回收率在86.4%~106%之间, 精密度为2.95%~5.37%, 方法检出限为0.002 mg/kg, 定量限为0.006 mg/kg。结论 该方法准确灵敏, 适合测定海洋贝类中无机镉离子。

英文摘要:

      Objective To establish a method for the determination of inorganic cadmium ions in marine shellfish by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Methods A certain amount of samples were added to the extract of 10 mmol/L Tris-HCl (0.1 mol/L NaCl solution was added), ultrasonic extraction for 2 h, centrifuged and filtered, and then tested on the machine in the sample bottle. The mobile phase was 30 mmol/L oxalic acid aqueous solution and 55 mmol/L potassium hydroxide aqueous solution. Cadmium ions were separated by CS5A cationic exchange chromatography column and CG5A protective column, and determined by inductively coupled plasma mass spectrometer. Results The method had a good linear relationship, r=0.998, recovery rate between 86.4% and 106%, precision between 2.95% and 5.37%, detection limit of the method was 0.002 mg/kg, and quantitative limit was 0.006 mg/kg. Conclusion This method is accurate and sensitive, suitable for the determination of inorganic cadmium ions in marine shellfish.