高效液相色谱-电感耦合等离子体质谱法测定不同膳食基质中5种砷形态的方法研究

Analysis of Five Arsenic Speciations by High Performance Liquid Chromatography and Inductively Coupled Plasma Mass Spectrometry

中文关键词:  总膳食  砷形态分析  高效液相色谱-电感耦合等离子体质谱

英文关键词:food  arsenic speciation analysis  high performance liquid chromatography and inductively coupled plasma mass spectrometry

中文摘要:

      目的：应用高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用技术优化完善不同膳食基质中五价砷(As5+)、砷甜菜碱(AsB)、三价砷(As3+)、二甲基砷酸(DMA)和一甲基砷酸(MMA)5种砷形态的检测方法。方法：通过比较不同浓度的乙酸、盐酸、硝酸水溶液在热提取条件下对不同膳食基质(谷类、饮料类、水产类、蛋类、豆类、水果类、糖类)及对NIST标准参考物质Rice Flour1568b中5种砷形态化合物的提取效果，确定最佳提取试剂最佳提取浓度，同时比较不同pH、不同流动相下砷化合物的分离效果，确定最终分离条件。结果：膳食样品中砷形态分析的最佳提取方法为0.15 mol/L硝酸水溶液浸泡提取；以20 mmol/L柠檬酸和5 mmol/L己烷磺酸钠的混合溶液为流动相（pH=4.3），5种砷形态的线性范围线0～100 μg/L相关系数（r）均大于0.999，检出限为0.4～1.2 μg/L，精密度好，RSD均小于5%。不同膳食样品(谷类、饮料类、水产类、蛋类、豆类、水果类、糖类)加标回收率为80%～113%(无机砷)、81%～122%(MMA)、80%～124% (DMA)、77%～120%(AsB)；采用本方法测定的NIST标准参考物质Rice Flour 1568b测定值跟标示值相吻合。结论：本实验优化了砷形态分析的前处理方法和分离条件，不仅具有省时、快速高效，仅4 min即可完成对五种砷形态的检测的优势，而且可以保证测定结果的准确性。

英文摘要:

      Objectives A high performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS) was established for analysis 5 arsenic speciations，including As5+, AsB, As3+, DMA and MMA. Methods By comparing the different concentrations of acetic acid, hydrochloric acid, nitric acid solution under the condition of thermal extract of different dietary matrix (grains, drinks, aquatic products, eggs, beans, fruits and sugar) and the NIST standard reference material of 5 arsenic speciations in Rice Flour1568b extraction effect, to determine the best extraction and concentration of reagents, at the same time to compare different pH, arsenic compounds under different mobile phase separation effect, the final separation conditions were determined. Results Arsenic speciation analysis in dietary samples the best extraction method is 0.15 mol/L nitric acid soak extract; On 20 mmol/L a mixture of citric acid and 5 mmol/L hexane sulfonic acid sodium solution as mobile phase (pH = 4.3), line of five different forms of arsenic linear range 0 to 100 μg/L, the correlation coefficient (r) were greater than 0.999, the detection limit of 0.4 ~ 1.2 μg/L, good precision, and RSD is less than 5% and the standard addition recovery was 80% ~ 113% (iAs), 81% ~ 122% (MMA), 80% ~ 124% (DMA), 77% ~ 120% (AsB); Using this method for determining the NIST standard reference material Rice Flour 1568 b measured value consistent with marked value. Conclusion This experiment optimized the arsenic speciation analysis methods of pretreatment and separation conditions, not only has the time-saving, fast and efficient, only 4 min was able to advantage of five different forms of arsenic detection, but also can ensure the accuracy of determination results.