原子荧光光谱法测定糙米粉中总砷及无机砷的含量

Determination of total arsenic and inorganic arsenic in brown rice flour by atomic fluorescence spectrometry

中文关键词:  砷  盲样考核  糙米粉  液相色谱-原子荧光光谱法

英文关键词:arsenic  blindness assessment  brown rice flour  atomic fluorescence spectrometry

中文摘要:

      目的 建立原子荧光光谱法测定糙米粉中总砷及无机砷含量的分析方法。方法 糙米粉经烘干称取后, 用硝酸高氯酸硫酸混合湿法消解快速进行总砷前处理, 用1%硝酸水浴热提取进行无机砷前处理, 分别利用原子荧光光谱法及液相色谱-原子荧光光谱法进行总砷和无机砷的测定。结果 总砷在6.0~20.0 μg/L浓度范围内, 无机砷在10.0~100.0 μg/L浓度范围内均具有良好的线性关系(r＞0.999), 大米粉质控样测定值总砷0.26 mg/kg及无机砷0.17 mg/kg, 均在参考值允许范围内, 回收率范围为92.3%~127.1%, 均具有较高的回收率。结论 优化湿法消解处理能较高效地得到准确的测定结果, 糙米粉中无机砷经热提取及流动相环节的优化后, 也可得满意检测结果。

英文摘要:

      Objective To establish a method for determination of total arsenic and inorganic arsenic in brown rice flour by atomic fluorescence spectrometry. Methods The brown rice flour was dried and weighed, and then the total arsenic pretreatment was quickly carried out by wet digestion with nitric acid, perchloric acid and sulfuric acid, and the inorganic arsenic pretreatment was carried out by hot extraction with a 1% nitric acid water bath. The total arsenic and inorganic arsenic was determined by atomic fluorescence spectrometry and liquid chromatography-atomic fluorescence spectrometry, respectively. Results Total arsenic and inorganic arsenic had a good linear relationship (r>0.999) in the range of 6.0?20.0 and 10.0?100.0 μg/L. The total arsenic content of 0.26 mg/kg and inorganic arsenic content of 0.17 mg/kg in the control sample of rice were within the allowable range of reference value, and the recovery rate was 92.3%?127.1%, both of which had higher recovery rates. Conclusion The optimized wet digestion treatment can obtain accurate measurement results more efficiently. After the hot extraction of inorganic arsenic in the brown rice flour and the optimization of the mobile phase, satisfactory results can be obtained.