【引用本文】 秦冲, 施畅, 万秋月, 等. 高效液相色谱-电感耦合等离子体质谱联用检测土壤中的无机硒形态[J]. 岩矿测试, 2018, 37(6): 664-670. doi: 10.15898/j.cnki.11-2131/td.201803200024
QIN Chong , SHI Chang , WAN Qiu-yue , et al. Speciation Analysis of Inorganic Selenium in Soil by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2018, 37(6): 664-670. doi: 10.15898/j.cnki.11-2131/td.201803200024

高效液相色谱-电感耦合等离子体质谱联用检测土壤中的无机硒形态

河北省地质实验测试中心, 河北 保定 071051

收稿日期: 2018-03-20  修回日期: 2018-07-09 

基金项目: 河北省地质矿产勘查开发局科技项目(201827)

作者简介: 秦冲,工程师,主要从事地质实验测试工作。E-mail:qinchong0013@163.com。。

通讯作者:

Speciation Analysis of Inorganic Selenium in Soil by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

Hebei Research Center for Geoanalysis, Baoding 071051, China

Corresponding author: SHI Chang , 主要从事地质实验测试工作。shichang1218@163.com。

Received Date: 2018-03-20
Revised Date: 2018-07-09

摘要:土壤样品中亚硒酸盐Se(Ⅳ)和硒酸盐Se(Ⅵ)的形态分析中,提取剂的选择和检测方法是技术的关键。以往的提取剂容易导致硒形态发生转变或无法同时提取Se(Ⅳ)和Se(Ⅵ),常用的氢化物发生原子荧光光谱法无法直接测定Se(Ⅵ),而是通过差减法得出Se(Ⅵ)含量。本文对比了不同提取剂的提取能力,确定使用0.1 mol/L氢氧化钠溶液作为提取剂,在55℃超声萃取土壤样品30 min,提取液经高效液相色谱分离,电感耦合等离子体质谱检测,建立了土壤中Se(Ⅳ)和Se(Ⅵ)的形态分析方法。采用Hamilton PRP X-100色谱柱,以6 mmol/L柠檬酸为流动相,pH=5.5,在8 min内可完全分离Se(Ⅳ)和Se(Ⅵ),两者的检出限分别为0.15 μg/L、0.16 μg/L,线性相关系数(r2)均大于0.999。以土壤为基体进行加标回收试验,Se(Ⅳ)和Se(Ⅵ)的回收率在84.2%~95.8%之间,相对标准偏差为1.4%~5.3%(n=6)。该方法简单快速,具有良好的精密度和准确度,适用于土壤中无机硒的形态分析。

关键词: 土壤, 亚硒酸盐, 硒酸盐, 氢氧化钠, 高效液相色谱-电感耦合等离子体质谱法

Speciation Analysis of Inorganic Selenium in Soil by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

KEY WORDS: soil, selenite, selenate, sodium hydroxide, High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

本文参考文献

[1]

Kápolna E,Fodor P.Speciation analysis of selenium enriched green onions (allium fistulosum) by HPLC-ICP-MS[J].Microchemical Journal,2006,84(1):56-62.

[2]

王丙涛,谢丽琪,林燕奎,等.高效液相色谱-电感耦合等离子体质谱联用检测食品中的五种硒形态[J].色谱,2011,29(3):223-227.

Wang B T,Xie L Q,Lin Y K,et al.Determination of selenium species in food by high performance liquid chromatography with inductively coupled plasma mass spectrometry[J].Chinese Journal of Chromatography,2011,29(3):223-227.

[3]

Uden P C,Boakye H T,Kahakachchi C,et al.Selective detection and identification of Se containing compounds-Review and recent developments[J].Journal of Chromatography A,2004,1050(1):85-93.

[4]

王欣,幸苑娜,陈泽勇,等.高效液相色谱-电感耦合等离子体质谱法检测富硒食品中6种硒形态[J].分析化学,2013,41(11):1669-1674.

Wang X,Xing Y N,Chen Z Y,et al.Determination of 6 selenium species in selenium-enriched food by hyphenated technique of high performance liquid chromatography-inductively coupled plasma mass spectrometry[J].Chinese Journal of Analytical Chemistry,2013,41(11):1669-1674.

[5]

Dumont E,Vanhaecke F,Cornelis R.Selenium speciation from food source to metabolites:A critical review[J].Analytical & Bioanalytical Chemistry,2006,385(7):1304-1323.

[6]

Połatajko A,Jakubowski N,Szpunar J.State of the art report of selenium speciation in biological samples[J].Journal of Analytical Atomic Spectrometry,2006,21(7):639-654.

[7]

邱建华,王秋泉,黄本立.硒形态分析研究进展[J].光谱学与光谱分析,2006,26(9):1692-1701.

Qiu J H,Wang Q Q,Huang B L.New approaches to selenium speciation[J].Spectroscopy and Spectral Analysis,2006,26(9):1692-1701.

[8]

B'Hymer C,Caruso J A.Selenium speciation analysis using inductively coupled plasma-mass spectrometry[J].Journal of Chromatography A,2006,1114(1):1.

[9]

Ogra Y,Anan Y.Selenometabolomics:Identification of selenometabolites and specification of their biological significance by complementary use of elemental and molecular mass spectrometry[J].Journal of Analytical Atomic Spectrometry,2009,24(11):1477-1488.

[10]

Rayman M P.Food-chain selenium and human health:Emphasis on intake[J].British Journal of Nutrition,2008,100(2):254-268.

[11]

Antanaitis A,Lubyte J,Antanaitis S,et al.Selenium con-centration dependence on soil properties[J].Journal of Food,Agriculture & Environment,2008,6(1):163-167.

[12]

Muchowski P.Assessing the speciation and the bioge-ochemical processes affecting the mobility of selenium from a geological repository of radioactive wastes to the biosphere[J].Analusis,1998,26(5):193-197.

[13]

Abrams M M,Burau R G,Zasoski R J.Organic selenium distribution in selected California soils[J].Soil Science Society of America Journal,1990,54(4):979-982.

[14]

Zhang Y,Moore J N.Selenium fractionation and spe-ciation in a wetland system[J].Environmental Science & Technology,1996,30(8):2613-2619.

[15]

Masscheleyn P H,Delaune R D,Patrick W H J.Transformations of selenium as affected by sediment oxidation-reduction potential and pH[J].Environmental Science & Technology,1990,24(1):91-96.

[16]

Masscheleyn P H,Delaune R D,Patrick W H.Arsenic and selenium chemistry as affected by sediment redox potential and pH[J].Journal of Environmental Quality,1991,20(3):522-527.

[17]

方金梅.福州市土壤硒形态分析及其迁移富集规律[J].岩矿测试,2008,27(2):28-32.

Fang J M.Selenium speciation analysis and its transformation and enrichment in soils of Fuzhou city[J].Rock and Mineral Analysis,2008,27(2):28-32.

[18]

徐强,迟凤琴,匡恩俊,等.基于通径分析的土壤性质与硒形态的关系——以黑龙江省主要类型土壤为例[J].土壤,2016,48(5):992-999.

Xu Q,Chi F Q,Kuang E J,et al.Relationship between soil physico-chemical properties and selenium species based on path analysis[J].Soils,2016,48(5):992-999.

[19]

Favorito J E,Luxton T P,Eick M J,et al.Selenium speciation in phosphate mine soils and evaluation of a sequential extraction procedure using XAFS[J].Environmental Pollution,2017,229:911-921.

[20]

耿建梅,王文斌,罗丹,等.不同浸提剂对海南稻田土壤有效硒浸提效果比较[J].土壤,2010,42(4):624-629.

Geng J M,Wang W B,Luo D,et al.Comparative studies on effects of several extractants on available selenium of paddy soils in Hainan[J].Soils,2010,42(4):624-629.

[21]

温国灿,黄艳,郭永玲,等.酸性土壤有效硒提取条件优化的研究[J].农业环境科学学报,2007,26(5):1996-2000.

Wen G C,Huang Y,Guo Y L,et al.Optimal conditions of extraction method for available selenium in acid soils[J].Journal of Agro-Environment Science,2007,26(5):1996-2000.

[22]

Wright M T,Parker D R,Amrhein C.Critical evaluation of the ability of sequential extraction procedures to quantify discrete forms of selenium in sediments and soils[J].Environmental Science & Technology,2003,37(20):4709-4716.

[23]

Stroud J L,McGrath S P,Zhao F J.Selenium speciation in soil extracts using LC-ICP-MS[J].International Journal of Environmental Analytical Chemistry,2012,92(2):222-236.

[24]

Zhang Y,Jr W T F.Determination of selenium frac-tionation and speciation in wetland sediments by parallel extraction[J].International Journal of Environmental Analytical Chemistry,2003,83(4):315-326.

[25]

Bujdoš M,Kubová J,Streško V.Problems of selenium fractionation in soils rich in organic matter[J].Analytica Chimica Acta,2000,408(1):103-109.

[26]

薛超群,郭敏.氢化物发生-原子荧光光谱法测定土壤样品中不同价态的硒[J].岩矿测试,2012,31(6):980-984.

Xue C Q,Guo M.Analysis of different valence states of selenium in geological samples by hydride generation-atomic fluorescence spectrometry[J].Rock and Mineral Analysis,2012,31(6):980-984.

[27]

彭岚,谈明光,李玉兰,等.微波辅助萃取-液质联用技术测底泥砷、硒的化学形态[J].分析试验室,2006,25(5):10-14.

Peng L,Tan M G,Li Y L,et al.Simultaneous speciation of arsenic and selenium by high-performance liquid chromatography on-line with inductively coupled plasma collision cell mass spectrometry in sediment samples[J].Chinese Journal of Analytical Laboratory,2006,25(5):10-14.

[28]

Hsieh Y J,Jiang S J.Determination of selenium com-pounds in food supplements using reversed-phase liquid chromatography-inductively coupled plasma mass spectrometry[J].Microchemical Journal,2013,110(9):1-7.

[29]

Zheng J,Ohata M,Furuta N,et al.Speciation of selenium compounds with ion-pair reversed-phase liquid chromatography using inductively coupled plasma mass spectrometry as element-specific detection[J].Journal of Chromatography A,2000,874(1):55-64.

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高效液相色谱-电感耦合等离子体质谱联用检测土壤中的无机硒形态

秦冲, 施畅, 万秋月, 王磊, 刘爱琴, 安彩秀