高效液相色谱-电感耦合等离子体质谱法测定土壤中6种砷形态  

Determination of six arsenic species in soil by high performance liquid chromatography-inductively coupled plasma mass spectrometry

作　　者：纪律[1] 汤鋆[2] 郑晨阳 李启[1] 谭莹[2] 胡争艳[2] JI Lv;TANG Jun;ZHENG Chen-yang;LI Qi;TAN Ying;HU Zheng-yan(Lishui Municipal Center for Disease Control and Prevention,Lishui,Zhejiang 323000,China;不详)

机构地区：[1]丽水市疾病预防控制中心,浙江丽水323000 [2]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2021年第20期2453-2457,共5页Chinese Journal of Health Laboratory Technology

基　　金：浙江省医药卫生科技计划项目(2021RC038)。

摘　　要：目的利用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术,建立土壤样品中亚砷酸根[As(Ⅲ)]、砷酸根[As(Ⅴ)]、一甲基砷(MMA)、二甲基砷(DMA)、砷甜菜碱(As B)和砷胆碱(As C) 6种砷形态的分析方法。方法样品以0.8 mol/L磷酸为提取液,常温超声辅助提取6 h后,采用Hamilton PRP-X100(4.1 mm×250 mm)阴离子交换色谱柱进行分离,以0.5 mmol/L碳酸铵+2%甲醇(p H=9.2)-50 mmol/L碳酸铵+8 mmol/L磷酸氢二氨+2%甲醇(p H值=9.2)为流动相进行梯度洗脱,于15 min内完成6种砷形态的分析测定。结果 6种砷形态在1μg/L~50μg/L浓度范围内线性良好,相关系数(r)均> 0.998,检出限为0.08μg/L~0.09μg/L,采用精密度考察方法重复性,相对标准偏差(RSD)为2.1%,除了亚砷酸根在磷酸溶液提取时完全进行了转化而无法测得加标回收率,其余回收率均在98.3%~109.6%。结论本方法适用于土壤样品中6种砷形态的测定,样品中检测到的砷形态总量占总砷含量的82.2%~94.1%,砷形态的提取率较高,结果较为满意。Objective To establish a method for the determination of 6 arsenic species including arsenite [As( Ⅲ) ],arsenate[As( Ⅴ) ],monmethyl arsenic( MMA),dimethyl arsenic( DMA),arsenobetaine( As B) and arsenocholine( As C) in soil by high performance liquid chromatography-inductively coupled plasma mass spectrometry( HPLC-ICP/MS). Methods The sample was ultrasonic extracted by 0. 8 mol/L phosphoric acid. Six arsenic species were detected in 15 min by Hamilton PRP-X100( 4. 1 mm × 250 mm) anion exchange column with 0. 5 mmol/L ammonium carbonate + 2% methanol( p H = 9. 2)-50 mmol/L ammonium carbonate + 8 mmol/L ammonium phosphate + 2% methanol( p H = 9. 2) as the mobile phase for gradientelution. Results The linear ranges for 6 arsenic species were between 1 μg/L-50 μg/L with the linear coefficients( r)more than 0. 998,and the detection limits were between 0. 08 μg/L-0. 09 μg/L. The repeatability of the method was examined by precision. The relative standard deviation( RSD) was 2. 1%. The recoveries ranged from 98. 3% to 109. 6%,except that arsenite was completely transformed during phosphoric acid extraction. Conclusion The method was suitable for the analysis and determination of arsenic species in soil. The ratio of the total amount of arsenic species to total arsenic in the sample is within 82. 2%-94. 1%. The extraction rate of arsenic species was higher and the result was satisfactory.

关 键 词：高效液相色谱-电感耦合等离子体质谱 土壤 砷 形态分析 

分 类 号：O657[理学—分析化学]