Determination of Selenium Content in Selenium-Enriched Polysaccharides by Dispersive Liquid-Liquid Microextraction Coupled to Reversed Phase High-Performance Liquid Chromatography with Fluorescence Detector

  • WANG Fengqin ,
  • CAO Jinping ,
  • LU Zeqing ,
  • WANG Yizhen
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  • Key Laboratory of Animal Feed and Nutrition of Zhejiang Province, Key Laboratory of Animal Nutrition and Feed Science(Eastern of China), Ministry of Agriculture and Rural Affairs, Feed Science Institute of Zhejiang University, Hangzhou 310058, China

Received date: 2020-07-08

  Online published: 2021-02-04

Supported by

 

Abstract

This study described a new method using dispersive liquid-liquid microextraction prior to reverse phase high-performance liquid chromatography with fluorescence detector (HPLC-FLD) on a new reversed-phase column for the determination of selenium content in selenium-enriched polysaccharides. In the procedure, 2,3-diaminonaphthalene (DAN) was used as the chelating reagent, 400 μL acetonitrile was used as the dispersive solvent and 120 μL chlorobenzene was used as the extraction solvent. The chelate of selenium (Ⅳ) and DAN (Se-DAN chelate) was diluted by acetonitrile and then was analyzed by high-performance liquid chromatography. Using acetonitrile as mobile phase, the Se-DAN chelate was separated by PFP column, and the fluorescence intensity was determined by fluorescence detector (excitation wavelength at 376 nm and emission wavelength at 520 nm) and quantitative analysis by external standard method. The sample was quantified by external standard method. The results showed that this method was successfully applied to determine the selenium content in selenium-enriched polysaccharides with the detection limit of selenium was 2.5 μg/L, and the linear range was 0.5 to 250.0 μg/L. In this experiment, a method for determination of selenium content in selenium-enriched polysaccharides is successfully set, and this method has the advantages of simple and fast operation, low reagent consumption and high recovery rate and good applicability.

Cite this article

WANG Fengqin , CAO Jinping , LU Zeqing , WANG Yizhen . Determination of Selenium Content in Selenium-Enriched Polysaccharides by Dispersive Liquid-Liquid Microextraction Coupled to Reversed Phase High-Performance Liquid Chromatography with Fluorescence Detector[J]. Chinese Journal of Animal Nutrition, 2021 , 33(2) : 1120 -1127 . DOI: 10.3969/j.issn.1006-267x.2021.02.052

References

[1] TINGGI U.Essentiality and toxicity of selenium and its status in Australia:a review[J].Toxicology Letters,2003,137(1/2):103-110.
[2] MUÑIZ-NAVEIRO Ó,DOMÍNGUEZ-GONZÁLEZ R,BERMEJO-BARRERA A,et al.Selenium speciation in cow milk obtained after supplementation with different selenium forms to the cow feed using liquid chromatography coupled with hydride generation-atomic fluorescence spectrometry[J].Talanta,2007,71(4):1587-1593.  
[3] VINCENT J L,FORCEVILLE X.Critically elucidating the role of selenium[J].Current Opinion in Anaesthesiology,2008,21(2):148-154.  
[4] NAVARRO-ALARCÓN M,LÓPEZ-MARTÍNEZ M C.Essentiality of selenium in the human body:relationship with different diseases[J].Science of the Total Environment,2000,249(1/2/3):347-371.
[5] ZACHARIADIS G A,KAPSIMALI D C,ROSENBERG E.A review of recent developments in sample pretreatment,separation and hyphenated atomic and mass spectrometric techniques for organoselenium speciation in biological liquids[J].Current Organic Chemistry,2010,14(19):2282-2299.  
[6] ABBAS-GHALEB K,GILON N,CRÉTIER G,et al.Preconcentration of selenium compounds on a porous graphitic carbon column in view of HPLC-ICP-AES speciation analysis[J].Analytical and Bioanalytical Chemistry,2003,377(6):1026-1031.  
[7] SELE V,ØRNSRUD R,SLOTH J J,et al.Selenium and selenium species in feeds and muscle tissue of Atlantic salmon[J].Journal of Trace Elements in Medicine and Biology,2018,47:124-133.
[8] SCHLOSKE L,WALDNER H,MARX F.Optimisation of sample pre-treatment in the HG-AAS selenium analysis[J].Analytical and Bioanalytical Chemistry,2002,372(5/6):700-704.
[9] MESTEK O,SUCHÁNEK M,VODIČKOVÁ Z,et al.Comparison of the suitability of various atomic spectroscopic techniques for the determination of selenium in human whole blood[J].Journal of Analytical Atomic Spectrometry,1997,12(1):85-89.  
[10] 林海兰,朱日龙,于磊,等.水浴消解-原子荧光光谱法测定土壤和沉积物中砷、汞、硒、锑和铋[J].光谱学与光谱分析,2020,40(5):1528-1533. LIN H L,ZHU R L,YU L,et al.Determination of arsenic,mercury,selenium,antimony and bismuth in soil and sediments by water bath digestion-atomic fluorescence spectrometry[J].Spectroscopy and Spectral Analysis,2020,40(5):1528-1533.(in Chinese)
[11] TIE M,LI B R,SUN T B,et al.HPLC-ICP-MS speciation of selenium in Se-cultivated Flammulina velutipes[J].Arabian Journal of Chemistry,2020,13(1):416-422.  
[12] ANDO M,TAKIZAWA M,SUWABE S,et al.Determination of selenium in human serum by liquid chromatography/electron capture atmospheric pressure chemical ionization mass spectrometry after acid digestion and derivatization using 2,3-diaminonaphthalene[J].European Journal of Mass Spectrometry,2003,9(6):619-622.  
[13] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13883-2008饲料中硒的测定[S].北京:中国标准出版社,2008. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China.GB/T 13883-2008 Determination of selenium in feeds[S].Beijing:China Standards Press,2008.(in Chinese)
[14] SHIBATA Y,MORITA M,FUWA K.Determination of selenium by liquid chromatography with spectrofluorometric detection[J].Analytical Chemistry,1984,56(8):1527-1530.  
[15] ZHOU Q X,LEI M,LI J,et al.Selenium speciation in tea by dispersive liquid-liquid microextraction coupled to high-performance liquid chromatography after derivatization with 2,3-diaminonaphthalene[J].Journal of Separation Science,2015,38(9):1577-1583.  
[16] 徐春兰.Enterobacter cloacae Z0206富硒多糖的制备、结构分析及其主要生物学功能研究[D].博士学位论文.杭州:浙江大学,2008:45-46. XU C L.Preparation,structural analysis and biological function research of selenium-enriched exopolysaccharide produced by bacterium Enterobacter cloacae Z0206[D].Ph.D.Thesis.Hangzhou:Zhejiang University,2008:45-46.(in Chinese)
[17] JIN M L,WANG Y M,XU C L,et al.Preparation and biological activities of an exopolysaccharide produced by Enterobacter cloacae Z0206[J].Carbohydrate Polymers,2010,81(3):607-611.  
[18] WANG F Q,YANG H X,WANG Y Z.Structure characterization of a fucose-containing exopolysaccharide produced by Enterobacter cloacae Z0206[J].Carbohydrate Polymers, 2013,92(1):503-509.  
[19] XU C L,WANG Y Z,JIN M L,et al.Preparation,characterization and immunomodulatory activity of selenium-enriched exopolysaccharide produced by bacterium Enterobacter cloacae Z0206[J].Bioresource Technology,2009,100(6):2095-2097.  
[20] 王凤芹,程远之,肖肖,等.高效液相色谱-电感耦合等离子体质谱法测定富硒蛋白多糖中纳米单质硒含量[J].动物营养学报,2018,30(3):1155-1161. WANG F Q,CHENG Y Z,XIAO X,et al.Measurement of nano elemental selenium in selenium-enriched polysaccharides using high performance liquid chromatography coupled with inductivity coupled plasma mass spectrometry method[J].Chinese Journal of Animal Nutrition,2018,30(3):1155-1161.(in Chinese)
[21] RAJAN M,BARBOSA F P,GUALBERTO N C,et al.Optimization and method validation of determining polyphenolic compounds by UFLC-DAD system using two biphenyl and pentafluorophenylpropyl columns[J].Journal of Liquid Chromatography & Related Technologies,2019,42(11/12):351-357.
[22] 罗辉泰,黄晓兰,吴惠勤,等.QuEChERS-同位素稀释-液相色谱-高分辨飞行时间质谱法高通量筛查化妆品中86种糖皮质激素[J].分析化学,2017,45(9):1381-1388. LUO H T,HUANG X L,WU H Q,et al.High throughput screening of 86 kinds of glucocorticoids in cosmetics using QuEChERS and isotope dilution-liquid chromatography copuled to high resolution time-of-flight mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(9):1381-1388.(in Chinese)
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