Analysis of Six Arsenic Speciations in Urine by High Performance Liquid Chromatography－Inductively Coupled Plasma Mass Spectrometry

LIU Yang; CHEN Shao-zhan; LIU Li-ping; LI Xiao-yu; LI Qian-yu

doi:10.19969/j.fxcsxb.22091504

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Analysis of Six Arsenic Speciations in Urine by High Performance Liquid Chromatography－Inductively Coupled Plasma Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-02-28

- Analysis of Six Arsenic Speciations in Urine by High Performance Liquid Chromatography－Inductively Coupled Plasma Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 2, Pages: 227-232(2023)
- 作者机构：
  
  1.北京市疾病预防控制中心，食物中毒诊断溯源技术北京市重点实验室，北京 100013
  2.首都医科大学公共卫生学院，北京 100069
  3.中国食品药品检定研究院，北京 100162
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22091504
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刘洋,陈绍占,刘丽萍等.高效液相色谱－电感耦合等离子体质谱法分析尿中6种砷形态[J].分析测试学报,2023,42(02):227-232.

LIU Yang,CHEN Shao-zhan,LIU Li-ping,et al.Analysis of Six Arsenic Speciations in Urine by High Performance Liquid Chromatography－Inductively Coupled Plasma Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(02):227-232.
刘洋,陈绍占,刘丽萍等.高效液相色谱－电感耦合等离子体质谱法分析尿中6种砷形态[J].分析测试学报,2023,42(02):227-232. DOI： 10.19969/j.fxcsxb.22091504.

LIU Yang,CHEN Shao-zhan,LIU Li-ping,et al.Analysis of Six Arsenic Speciations in Urine by High Performance Liquid Chromatography－Inductively Coupled Plasma Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(02):227-232. DOI： 10.19969/j.fxcsxb.22091504.

摘要

采用高效液相色谱－电感耦合等离子体质谱法（HPLC－ICP－MS）分析人尿中砷甜菜碱（AsB）、二甲基砷（DMA）、砷胆碱（AsC）、亚砷酸盐（As（Ⅲ））、一甲基砷（MMA）、砷酸盐（As（V））6种砷形态。样品经水稀释后，采用Dionex IonPac As7阴离子交换色谱柱为分析柱，20 mmol/L碳酸铵（2%甲醇）和100 mmol/L碳酸铵（含2%甲醇）为流动相，梯度洗脱，HPLC－ICP－MS分析砷形态。6种砷形态在0 ~ 100 μg/L范围内线性关系良好，相关系数（,r,）均大于0.999，检出限为0.05 ~ 0.15 μg/L，不同浓度水平砷形态的相对标准偏差（RSD）均小于5.0%。3种不同浓度水平的加标回收率为91.8% ~ 108%，有证标准物质“冷冻人尿中砷形态”（NIST SRM 3669）中5种砷形态的测定结果在标准值范围内。实验结果表明，该方法准确可靠、灵敏度高、分析时间短，适用于人尿中砷形态的分析测定。同时研究了食用不同含砷食物后尿中砷形态的种类，结果显示不同的含砷食品，其砷在人体内的代谢转化不同。

Abstract

A high performance liquid chromatography－inductively coupled plasma mass spectrometry（HPLC－ICP－MS） was developed for the analysis of six arsenic speciations，i.e．arsenic betaine（AsB），dimethyl arsenic（DMA），arsenic choline（AsC），arsenite（As（Ⅲ）），monomethyl arsenic（MMA） and arsenate（As（V）） in human urine．After the samples were diluted with water，the arsenic speciations were separated on a Dionex IonPac As7 anion exchange column by gradient elution，with 20 mmol/L ammonium carbonate（2% methanol） and 100 mmol/L ammonium carbonate（2% methanol） as the mobile phase，and finally analyzed by HPLC－ICP－MS．The results indicated that the linear ranges for six arsenic speciations were all between 0 μg/L and 100 μg/L，with their correlation coefficients（,r,） more than 0.999．The detection limits were between 0.05 μg/L and 0.15 μg/L．The reproducibility of this method was evaluated by precision under different concentrations，with relative standard deviations（RSDs） less than 5.0%．The recoveries for six arsenic speciations at three spiked levels ranged from 91.8% to 108%．The evaluation results for five arsenic speciations in the standard reference material－Arsenic Species in Frozen Human Urine（NIST SRM 3669） were all within the range of standard values．This method was sensitive，rapid，reproducible and accurate，and it was suitable for rapid determination of arsenic speciations in human urine．The arsenic species in human urine were also characterized after food consumption．It was revealed that different metabolic transformations occurred in human body after different foods containing arsenic were consumed.

关键词

尿砷形态高效液相色谱－电感耦合等离子体质谱法

Keywords

urinearsenic speciationhigh performance liquid chromatography－inductively coupled plasma mass spectrometry

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广东省职业病防治院

、中国刑事警察学院刑法医系

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上海海洋大学食品学院

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