| 土壤中形态砷的高效液相色谱-氢化物发生-原子荧光测定方法 |
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| 引用本文： | 刘佩佩,梅勇,宋冠仪,商律,姬晓宇.土壤中形态砷的高效液相色谱-氢化物发生-原子荧光测定方法[J].现代预防医学,2016,0(24):4500-4502. |
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| 作者姓名： | 刘佩佩 梅勇 宋冠仪 商律 姬晓宇 |
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| 作者单位： | 武汉科技大学公共卫生学院，湖北 武汉 430065 |
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| 摘 要： | 目的 建立土壤中形态砷的高效液相色谱-氢化物发生-原子荧光光谱分析方法。方法 采用磷酸-盐酸混合浸提体系和超声振荡提取土壤中不同形态的砷。阴离子交换柱分离，高效液相色谱-氢化物发生-原子荧光光谱法测定，保留时间定性，峰面积定量。结果 该方法线性相关系数均大于0.999。三价砷、五价砷、一甲基砷和二甲基砷的测定范围分别为0.5 mg/kg～28.0 mg/kg、1.2 mg/kg～21.0 mg/kg、0.3 mg/kg～20.8 mg/kg和0.6 mg/kg～29.2 mg/kg。平均回收率达到96.2%～101.6%，日内精密度（RSD）≤3.7%，日间精密度（RSD）≤6.5%。3种污泥土壤样品均检测到三价砷和一甲基砷，浓度范围分别为1.3 mg/kg～6.2 mg/kg和3.7 mg/kg～9.1 mg/kg之间，五价砷和二甲基砷均低于检测限。结论 本法灵敏、准确、精密度好，适于土壤中砷的形态分析。
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| 关 键 词： | 砷形态 土壤 高效液相色谱法 氢化物发生 原子荧光光谱法 |
Determination of arsenic in soil by HPLC-hydride generator-AFS |
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| LIU Pei-pei,MEI Yong,SONG Guan-yi,SHANG Lv,JI Xiao-yu.Determination of arsenic in soil by HPLC-hydride generator-AFS[J].Modern Preventive Medicine,2016,0(24):4500-4502. |
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| Authors: | LIU Pei-pei MEI Yong SONG Guan-yi SHANG Lv JI Xiao-yu |
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| Affiliation: | School of Public Health, Wuhan University of Science and Technology, Wuhan, Hubei 430065, China |
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| Abstract: | Objective The study aimed to establish an analytic method for determination of arsenic in soil by high performance liquid chromatography (HPLC) coupled with hydride generator and atomic fluorescence spectrometry. Methods Arsenic of different forms was obtained by soaking in and extraction with phosphoric acid-hydrochloric acid mixture, followed by ultrasonic oscillation and purification through an anion exchange column. The sample was examined by HPLC-hydride generator-atomic fluorescence spectrometry, qualitized according to the retention time, and quantitized according to the peak areas. Results Linear correlation coefficients of the method were over 0.999. The detection ranges of trivalent arsenic, pentavalent arsenic, monomethylated arsenic, and dimethylated arsenic were 0.5 mg/kg-28.0 mg/kg, 1.2 mg/kg-21.0 mg/kg, 0.3 mg/kg-20.8 mg/kg, and 0.6 mg/kg-29.2 mg/kg, respectively. The average recovery rate reached 96.2%-101.6%, the intraday precision (RSD) was ≤ 3.7%, and the interday precision (RSD) was ≤ 6.5%. Trivalent arsenic and monomethylated arsenic were detected in all 3 sludge soil samples, and the concentrations fell within the ranges of 1.3 mg/kg-6.2 mg/kg and 3.7 mg/kg-9.1 mg/kg respectively. Pentavalent arsenic and dimethyl arsenic were both lower than the detection limits. Conclusion The method is sensitive, accurate, and high in precision, and is suitable for analyzing the distribution of different arsenic forms in soil. |
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| Keywords: | Arsenic form Soil High Performance Liquid Chromatography (HPLC) Hydride generator Atomic fluorescence spectrometry |
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