Ma Caijuan, Ouyang Peipei, Zheng Qianqing, Qiu Fubao
Zhongshan Center for Disease Control and Prevention, Zhongshan, Guangdong Province, 528403, China.
Anal Methods. 2025 Jul 10;17(27):5726-5735. doi: 10.1039/d5ay00204d.
A method for the rapid separation and detection of dimethylarsenate (DMA), arsenite [As(iii)], monomethylarsenate (MMA), and arsenate [As(v)] was developed. This method combined high performance liquid chromatography with atomic fluorescence spectrometry (HPLC-AFS) pressure tank-assisted extraction. Key parameters, including extraction temperature, extraction time, and extraction liquid concentration, were systematically investigated. Through orthogonal testing of the three factors at three levels, the optimal extraction conditions were identified as a nitric acid solution concentration of 1%, an extraction temperature of 150 °C, and an extraction time of 75 min. The results demonstrated that the four arsenic species could be completely separated within 6 min. Good linear relationships were observed in the concentration range of 1.00-100.0 μg L for all species, with detection limits ranging from 0.21 to 0.85 μg L. The recoveries were between 88.6% and 103%, with relative standard deviations ranging from 1.4% to 4.8%. The method was successfully applied to detect the concentrations of arsenic species in dried seafood products, and it yielded satisfactory results. Moreover, the total arsenic concentration was quantified using atomic fluorescence spectrometry after wet digestion. The total concentration of arsenic in the samples was between 4.22 mg kg and 24.4 mg kg, and the extraction efficiency, calculated as the percentage of the total arsenic species content extracted by the method to the total arsenic concentration, ranged from 1.35% to 13.5%. Notably, the inorganic arsenic levels in the analyzed samples were below the established safety limits.
开发了一种快速分离和检测二甲基砷酸盐（DMA）、亚砷酸盐[As(iii)]、一甲基砷酸盐（MMA）和砷酸盐[As(v)]的方法。该方法将高效液相色谱与原子荧光光谱法（HPLC-AFS）和压力罐辅助萃取相结合。系统研究了萃取温度、萃取时间和萃取液浓度等关键参数。通过对这三个因素进行三水平的正交试验，确定最佳萃取条件为硝酸溶液浓度1%、萃取温度150℃、萃取时间75分钟。结果表明，这四种砷形态可在6分钟内完全分离。所有形态在1.00 - 100.0 μg/L浓度范围内均呈现良好的线性关系，检测限为0.21至0.85 μg/L。回收率在88.6%至103%之间，相对标准偏差为1.4%至4.8%。该方法成功应用于检测干海产品中砷形态的浓度，并获得了满意的结果。此外，采用湿法消解后用原子荧光光谱法对总砷浓度进行了定量。样品中总砷浓度在4.22 mg/kg至24.4 mg/kg之间，该方法萃取的总砷形态含量占总砷浓度的百分比计算得出的萃取效率在1.35%至13.5%之间。值得注意的是，分析样品中的无机砷水平低于既定的安全限值。
