HPLC-ICP-MS法同时测定贝类中5种砷形态化合物

采用水-甲醇(1:1,V/V)溶液超声波辅助萃取,建立了同时快速测定贝类中砷胆碱、砷甜菜碱、亚砷酸、砷酸和4-氨基苯胂酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。对萃取溶液浓度、超声波辅助萃取温度和时间等条件进行了优化。选用Hamilton PRP-X100阴离子分析柱,以50 mmol/L碳酸铵-甲醇(99:1,V/V)溶液为流动相,进行梯度洗脱对5种砷形态分离,并优化了质谱测试条件。试验结果表明,5种砷形态达到很好的分离效果,在质量浓度为0~100μg/L的范围内与其对应的峰面积均具有良好的线性关系,线性相关系数r²均大于0.999,检出限在0.2~0.60μg/L之间,两水平样品加标回收率在90.5%~103.5%之间,方法的精密度在1.6%~4.2%之间。

Simultaneous Determination of 5 Arsenic Species in Shellfish by HPLC-ICP-MS

A method was developed for the simultaneous and rapid determination of arsenic choline,arsenic betaine,arsenous acid,arsenic acid and 4-aminophenylarsonic acid in shellfish through high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS),with samples extraction by oscillating in water-methanol(1:1,V/V).The concentration of extraction solution,ultrasonic-assisted extraction temperature and time were optimized.An anion-exchange column(Hamilton PRP-X100)was found suitable the simultaneous separation inorganic and organic species.Five compounds were separated using 50 m mol/L(NH4)2CO3-methanol(99:1,V/V)with a gradient elution,and ICP-MS conditions was optimized.The results showed that the five kinds of arsenic species can reach the baseline separation,and the arsenic concentration in the range of 0-100μg/L is linear,with correlation coefficients(r²)of all more than 0.999,and the detection limit was from 0.2μg/L to 0.6μg/L.The two levels of sample standard addition recovery rate range from 90.5%to 103.5%,the precision of the method is between 1.6%to 4.2%.