何易, 刘兰侠, 薛黎明, 熊丽蓓, 方亚敏. 高效液相色谱-电感耦合等离子体质谱法测定人尿中6种砷形态化合物[J]. 上海预防医学, 2023, 35(2): 182-186. DOI: 10.19428/j.cnki.sjpm.2023.22316
引用本文: 何易, 刘兰侠, 薛黎明, 熊丽蓓, 方亚敏. 高效液相色谱-电感耦合等离子体质谱法测定人尿中6种砷形态化合物[J]. 上海预防医学, 2023, 35(2): 182-186. DOI: 10.19428/j.cnki.sjpm.2023.22316
HE Yi, LIU Lanxia, XUE Liming, XIONG Libei, FANG Yamin. Determination of six arsenic species in human urine by HPLC-ICP-MS[J]. Shanghai Journal of Preventive Medicine, 2023, 35(2): 182-186. DOI: 10.19428/j.cnki.sjpm.2023.22316
Citation: HE Yi, LIU Lanxia, XUE Liming, XIONG Libei, FANG Yamin. Determination of six arsenic species in human urine by HPLC-ICP-MS[J]. Shanghai Journal of Preventive Medicine, 2023, 35(2): 182-186. DOI: 10.19428/j.cnki.sjpm.2023.22316

高效液相色谱-电感耦合等离子体质谱法测定人尿中6种砷形态化合物

Determination of six arsenic species in human urine by HPLC-ICP-MS

  • 摘要:
    目的 建立高效液相色谱-电感耦合等离子体质谱(HPLC⁃ICP⁃MS)测定人尿中砷胆碱(AsC)、砷甜菜碱(AsB)、三价砷(As3+)、二甲基砷酸(DMA5+)、甲基砷酸(MMA5+)、五价砷(As5+)等6种砷形态化合物含量的方法。
    方法 优化流动相pH值及无水乙醇含量,以50 mmol·L-1的(NH42CO3溶液(含2%无水乙醇、pH=8.5)为流动相,用He模式消除氯离子(Cl-)干扰,通过Hamilton PRP X⁃100阴离子交换色谱柱对 10倍稀释的人尿砷形态化合物进行分离,与ICP⁃MS联用,建立6种砷形态化合物的检测方法。
    结果 6种砷形态化合物13 min左右可以得到完全分离,标准曲线线性相关系数为0.999,检出限为0.10~0.20 μg·L-1,定量限为0.30~0.50 μg·L-1。精密度实验显示,加标浓度0.20 μg·L-1时相对标准偏差(RSD)为5.96%~9.07%;加标浓度2.00 μg·L-1时RSD为2.48%~6.38%,加标浓度5.00 μg·L-1时RSD为1.41%~2.57%。准确度实验显示,加标回收率为80%~125%。
    结论 所建立HPLC⁃ICP⁃MS测定人尿6种砷形态化合物的方法,快速、准确、灵敏,可应用于人群尿砷的测定。

     

    Abstract:
    Objective To establish an High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry (HPLC-ICP-MS) method for determination of six arsenic species in human urine,including arseniccholine (AsC), arsenobetaine (AsB), arsenite (As3+), dimethylarsinic acid (DMA5+), monomethylarsonic acid (MMA5+), and arsenate (As5+).
    Methods The pH value of mobile phase and the content of anhydrous ethanol were optimized. Ammonium carbonate (50 mmol·L-1, containing 2% anhydrous ethanol, pH-8.5) mobile phase was selected. Cl- interference was eliminated by He mode. The arsenic species in 10-fold diluted human urine samples were separated by an Hamilton PRP X-100 anionic column. A method for the determination of six arsenic species was established.
    Results Six arsenic species could be separated in 13 minutes. The linear correlation coefficients were above 0.999. The limits of detection were 0.10‒0.20 μg·L-1, and the limits of quantification were 0.30‒0.50 μg·L-1. Precision experiments showed that RSD ranged from 5.96% to 9.07% when adding concentration 0.20 μg·L-1; from 2.48% to 6.38% when adding concentration 2.00 μg·L-1; and from 1.41% to 2.57% when adding concentration 5.00 μg·L-1. Accuracy test showed that the recoveries were 80%‒125%.
    Conclusion The established HPLC-ICP-MS method for determination of six arsenic species in human urine is rapid, accurate and sensitive. It can be applied to the determination of arsenic species in human urine.

     

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