Keywords
Arsenic, Ion Exchange, Rice, Inorganic Arsenic
Abstract
Objective To establish an efficient and sensitive detection method for inorganic arsenic using new ion exchange column technology and detect the arsenic content in rice matrix. The method is based on a new ion exchange column. The pretreatment method, liquid phase separation and mass spectrometry measurement conditions for the analysis of inorganic arsenic in rice are optimized. Finally, the arsenic form compounds are separated by a new ion exchange column and a liquid chromatography-inductively coupled plasma mass spectrometry method. Perform testing. The external standard method was used for quantification, and the detection limit, precision and accuracy of the method were evaluated by detecting the content of arsenic form compounds in rice samples and rice standard samples. At the same time, 3 types of commercially available rice in Guangdong were selected as experimental samples for this study. 1 g of each sample was weighed and measured three times in parallel. This method was compared with the liquid chromatography-atomic fluorescence spectrometry (LC-AFS) in the national standard. , liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS) for comparison. The results were tested and found that when inorganic arsenic was extracted from rice with 0.5% nitric acid solution in a 65¡ãC ultrasonic water bath for 1.5 hours and the pH was adjusted to alkaline, the average extraction efficiency of rice was the highest (>93%). Use mobile phase A (8 mmol/L HNO 3, 50 mmol/L NH 3¡¤H 2O) and mobile phase B (40 mmol/L HNO 3, 80 mmol/L NH 3¡¤H 2O) as mobile phases for gradient elution. , under the measurement conditions of RF power 1500 W and atomization gas flow rate 0.97 L/min, the five arsenic form compounds can achieve baseline separation, and the detection limit range is 0.114~0.331 ¦Ìg/L. The inorganic arsenic content in the rice sample is 0.063~0.232 mg/kg, the results of measuring arsenic form compounds in rice flour standard material are all within the labeled uncertainty range, the recovery rate of standard addition is 86.7%~106.7%, and the measurement precision is 1.9%~12.5% respectively. Compared with the national standards, the measurement results of arsenate in rice are relatively close. The arsenate content of rice sample 1 detected by this study, LC-AFS, and LC-ICP-MS were 0.231, 0.226, and 0.236 mg/kg respectively. , and the national standard method is difficult to detect low-content arsenic form compounds due to insufficient sensitivity (arsenic betaine was not detected in rice sample 1). The method can detect the arsenic betaine content in rice sample 1 to be 0.023 mg/kg. Conclusion The method established in this study can meet the needs for the measurement of inorganic arsenic in rice. Compared with the current national standard, it can greatly shorten the detection time and improve the efficiency. It also reduces the method detection limit and improves the method sensitivity.
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Original research done by Yang Xingfen, Wang Jing, Hu Shuguang, Su Zujian, Fan Jianbin, Cai Wenhua, Huang Weixiong, Huang Hongyao
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