高效液相色谱-电感耦合等离子体质谱法测定食品中无机砷含量

Determination of inorganic arsenic in food by high performance liquid chromatography inductively coupled plasma mass spectrometry

中文关键词:  液相色谱-电感耦合等离子体质谱仪  无机砷  三价砷  五价砷

英文关键词:liquid chromatography inductively coupled plasma mass spectrometery, inorganic arsenic  trivalent arsenic  pentavalent arsenic

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测定食品中无机砷的分析方法。方法 样品用 20 mL 0.15 mol/L的硝酸溶液于90 ℃恒温箱中浸提2.5 h, 经8000 r/min离心15 min, 经Agileng Zobarx Column色谱柱分离, 以5 mmol/L己烷磺酸钠和20 mmol/L柠檬酸(用氢氧化钠调pH至4.3)为流动相。电感耦合等离子体质谱仪进行定量分析无机砷的含量。结果 三价砷和五价砷在1.0～50.0 μg/L浓度范围线性关系良好, 线性相关系数(r2)分别为0.9998和1.000; 三价砷的加标回收率为91%～108%, 相对标准偏差为1.5%～4.3%; 五价砷的加标回收率为85%～106%, 相对标准偏差为2.4%～6.4%。结论 该方法准确、灵敏, 适合于批量食品中无机砷含量的精确测定。

英文摘要:

      Objective To establish an analytical method for the determination of inorganic arsenic in food by high performance liquid chromatography-inductively coupled plasma mass spectrometry. Methods The sample was extracted by 20 mL 0.15 mol/L nitric acid solution in a 90 ℃ incubator for 2.5 h, centrifuged for 15 min at 8000 r/min, and separated by Agileng Zobarx column using 5 mmol/L sodium hexane sulfonate and 20 mmol/L citric acid (pH adjusted to 4.3 with sodium hydroxide) as mobile phase. The content of inorganic arsenic was quantitatively analyzed by inductively coupled plasma mass spectrometery. Results Trivalent arsenic and pentavalent arsenic had a good linear relationship in the concentration range of 1.0 to 50.0 μg/L, the linear correlation coefficients (r2) were 0.9998 and 1.000, respectively. The standard recovery rates of arsenic trivalent were 91%–108%, and the relative standard deviations were 1.5%–4.3%. The standard recovery rates of pentavalent arsenic were 85%–106%, and the relative standard deviations were 2.4%–6.4%. Conclusion The method is accurate, sensitive and suitable for the accurate determination of inorganic arsenic content in bulk food.