University of North Florida
Browse the Citations
-OR-

Contact Info

Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

View Stuart Chalk's profile on LinkedIn

Amit Chatterjee

Abbrev:
Chatterjee, A.
Other Names:
Address:
Environmental Chemistry Division, Environmental Chemodynamics Section, National Institute for Environmental Studies, 16-2 Onogawa, Ibaraki 305 0053, Tsukuba, Japan
Phone:
+1 302 831 4095
Fax:
+1 302 831 8525

Citations 9

"Determination Of Selenomethionine By High Performance Liquid Chromatography-direct Hydride Generation-atomic Absorption Spectrometry"
Microchem. J. 2001 Volume 69, Issue 3 Pages 179-187
Amit Chatterjee, Y. Shibata and M. Morita

Abstract: A simple, reliable, trace determination of selenomethionine (Semet) based on a direct hydride generation atomic absorption spectrometric method was developed using sodium tetralrydroborate (0.3% in 0.2% NaOH) and hydrochloric acid (3 M). The method excluded any chemical pretreatment prior to hydride generation (HG). The optimized HG system was successfully coupled with the HPLC system. The detection limit (3s, of blank; n = 5), reproducibility (RSD of three successive analyzes/day, performed on three different days), and repeatability (RSD of three successive analyzes) of the method were 1.08 ng mL-1, 9.8% for 9.04 ng mL-1 and 2.1-9.5% for 30.0-1.27 ng mL-1 Semet as Se (standards prepared in Milli-Q water). Calibration graph was linear up to 30 ng mL-1. This HPLC-HG-AAS method is very promising and successfully determined Semet (spiked) in human urine. (C) 2001 Elsevier Science B.V. All rights reserved.
Speciation

"High-performance Liquid Chromatography-ultrasonic Nebulizer High-power Nitrogen Microwave-induced Plasma Mass Spectrometry, Real-time On-line Coupling For Selenium Speciation Analysis"
J. Chromatogr. A 2004 Volume 1042, Issue 1-2 Pages 99-106
Amit Chatterjee, Yasuyuki Shibata, Hiroaki Tao, Atsushi Tanaka and Masatoshi Morita

Abstract: The coupling of a high-power nitrogen (N2) microwave-induced plasma (MIP) mass spectrometry - (MS) (1.3 kW) with high-performance liquid chromatography, connected with concentric nebulizer (CN), ultrasonic nebulizer (USN) and a hydride generation (HG) systems, for the optimization and determination of selenium compounds, has been carried out. The MIP-MS system fulfils the ideal requirement being an on-line real-time chromatographic detector for Se speciation analysis. Interchanging of MIP-MS system fabricated nebulizer (concentric) with an ultrasonic nebulizer increases about 3.4-12 (peak height) and 6.5-10 (peak area) times ion signals for the selenium compounds. The detection limits for selenate, selenite, trimethylselenonium ion (TmSe), selenomethionine (Semet) and selenoethionine (Seet) (in Milli-Q-water) obtained with the optimized HPLC-USN-N2MIP-MS system are 0.11, 0.14, 0.09, 0.14 and 0.10 µg L-1, respectively, about 12-48 times lower than the HPLC-CN-MIP-MS and 1.5-4.4 (peak height) times lower compared to the HPLC-CN-inductively coupled plasma (ICP)-MS coupling. Considering peak area, the repeatability (RSD for three successive analyzes) and intermediate precision (RSD for three successive analyzes performed on three different days), achieved for five Se compounds are 0.8-5.6, and 1.1-5.9%, comparable with the HPLC-CN-ICP-MS, HPLC-HG-MIP-MS and HPLC-CN-MIP-MS systems. The combined HPLC-USN-N2MIP-MS has been adequately applied for the determination of Se compounds in certified National Institute for Environmental studies human urine CRM No. 18. The results reasonably agree with the HPLC-CN-ICP-MS values. This encouraging combination may be an alternative ion source of mass spectrometry for coming generation in regard to the selenium speciation analysis.

"Determination Of Selenite And Selenomethionine By HPLC-HG-high Power N-2-MIP-MS: A Suitable Coupling For Selenium Speciation"
J. Anal. At. Spectrom. 2000 Volume 15, Issue 8 Pages 913-919
Amit Chatterjee, Yasuyuki Shibata and Masatoshi Morita

Abstract: The coupled technique, high performance liquid chromatography (HPLC) continuous hydride generation [flow-cell, with sodium tetrahydroborate (0.3% in 0.2% NaOH) and hydrochloric acid (3 M)] high power nitrogen microwave induced plasma [1.3 kW; 2.45 GHz, with an Okamoto cavity in a surface- wave mode (rectangular waveguide; WRJ-2)] mass spectrometry (N-2-MIP-MS) has been investigated for selenite and selenomethionine (Semet) determination. The high power N-2-MIP-MS was successfully coupled with a HG system that is attached with a PRP- x 100 anion exchange column. It was studied as an element specific detector for the optimization and determination of selenite and Semet using the major isotope of selenium (m/z 80). The adjusted HG system was very promising for the direct determination of the selenite and Semet without derivatization prior to HG. The N-2-MIP was stable in coupling with the HG system. The separation was performed with a phosphate buffer (15 mM at pH 7.0), which showed minimum suppression of volatile hydride formation from Semet among the mobile phases examined. The recovery of Semet (98-104%), prepared in the phosphate mobile phase, was almost same as that of Semet prepared in Milli-Q water. The detection limits of selenous acid and Semet obtained with the optimized HPLC-HG-N-2-MIP-MS system were 0.73 and 8.7 µg L-1, respectively. The repeatability (RSD for three successive analyzes) achieved for selenous acid and Semet were within 2.3-5.2%. The combined HPLC-HG-N-2-MIP-MS was applied to the determination of selenium compounds in human urine. The separation of selenite and Semet (spiked) in human urine was reasonable. The concentration of selenite found in the human urine was 3.7±0.2 µg L-1 which agreed well with the HPLC-ICP-MS value (3.8±0.2 µg l-1). Furthermore, in urine the retention times of selenite and Semet were shifted towards the solvent front. The spectroscopic interference due to calcium was removed.

"Estimation Of Arsenobetaine In The NIES Candidate Certified Reference Material No. 18 Human Urine By HPLC-ICP-MS Using Different Chromatographic Conditions"
Appl. Organomet. Chem. 2001 Volume 15, Issue 4 Pages 306-314
Amit Chatterjee, Yasuyuki Shibata, Jun Yoshinaga, Masatoshi Morita

Abstract: HPLC-ICP-MS, employing a silica-based LCSCX cation-exchange column, styrene-divinyl-benzene copolymer-based PRP- x 100 anion exchange column, an ODS reversed-phase and gel-permeation (polyvinyl alcohol-based resin) GS-220 columns, has been used for the separation, identification, and quantification of arsenic compounds, particularly arsenobetaine (AB), present in NIES candidate certified reference material (CRM) number 18 human urine. AB is the predominant arsenic species, followed by dimethylarsinic acid, methylarsonic acid and arsenic acid. The peak of each arsenic compound has been validated by spiking of the authentic standard solution to the urine sample and by using the above chromatographic systems. The high concentration of chloride that co-elutes with the arsenic acid from the LC-SCX and with the AB from the GS-220 columns has interfered with the ion signals of arsenic acid and AB, by forming the molecular ions (ArCl+)-Ar-40-Cl-35 and (ArCl+)-Ar-38-Cl-37 in the plasma. Thus, the concentration of AB has been carefully estimated on the GS-220 after extracting the chloride interference (Cl-37:Cl-35= 1:3.1271) by measuring the (ArCl+)-Ar-40-Cl-37. The peak of AB overlapped with the peak of arsenous acid and hindered the estimation of AB on the ODS and PRP- x 100 columns. But AB has been baseline separated from the other arsenic compounds and also from the chloride with 20 mM pyridine at pH 2.60 on the LC-SCX, So, the LC-SCX column has been proven and used for the determination of AB in NIES candidate CRM number 18 human urine. The concentrations of AB, estimated by the standard addition method and found using the LC-SCX and GS-220 columns, are 70.5±5.5 (n = 20) and 71.5±4 µg L-1 (n = 9), The concentration of AB thus found has been applied as the baseline value for the collaborative study to certify the AB in the NIES candidate CRM number 18 human urine.

"Identification Of Volatile Selenium Compounds Produced In The Hydride Generation System From Organoselenium Compounds"
Anal. Chem. 2001 Volume 73, Issue 13 Pages 3181-3186
Amit Chatterjee, Yasuyuki Shibata, Minoru Yoneda, Rupendranath Banerjee, Masao Uchida, Hiroyuki Kon, and Masatoshi Morita

Abstract: We report a novel aqueous derivatization of selenomethionine (Semet), selenoethionine (Seet) and trimethylselenonium ion (TmSe) by NaBH4 and HCl to volatile selenium species, namely, diethyldiselenide (DeDSe), dimethyldiselenide (DMDSe), dimethylselenide (DmSe) and ethylhydrogenselenide (ESeH), in the hydride generation (HG) system. The volatile selenium compounds produced in the HG system were on-line trapped and concentrated in a U-tube that was immersed in the liquid nitrogen trap. The trapped volatile Se compounds were volatilized at 80°C in a water bath, and 50-500 µL of volatile gas was injected into the GC/AED and GC/MS, respectively. It has been established that DmSe, DmDSe, and DeDSe are the predominant Se compounds that are produced in the HG system from TmSe, Semet, and Seet, respectively, followed by ESeH from Seet, Analytical methods previously employed have stated that these compounds are inactive in the HG system, Prior decomposition of Semet, Seet, and TmSe to selenous acid is essential before HG. To the best of our knowledge, current findings for the production and identification of volatile selenium compounds in the HG system are new and different from existing reports; hence, direct estimation of Semet, Seet, and TmSe is possible when coupling with a HG system using a suitable Se-specific detector.
Speciation

"Determination Of Arsenic Compounds By High-performance Liquid Chromatography-ultrasonic Nebulizer-high Power Nitrogen-microwave-induced Plasma Mass Spectrometry: An Accepted Coupling"
Anal. Chem. 2000 Volume 72, Issue 18 Pages 4402-4412
Amit Chatterjee, Yasuyuki Shibata, Jun Yoshinaga, and Masatoshi Morita

Abstract: To establish a sensitive, accurate, and precise determination of arsenic compounds, a high power nitrogen microwave-induced plasma (1.3 kW) mass spectrometer (N-2-MIP-MS) has been successfully coupled with an ultrasonic nebulizer (HPLC-USN) that is attached to a high-performance liquid chromatograph. It is examined as an element-specific detector for its applicability to the optimization and determination of seven arsenic compounds [arsenic acid, methylarsonic acid(MA), dimethylarsinic acid (DMA), arsenobetaine (AB), arsenocholine (AC), trimethylarsine oxide (TMAO), and tetramethylarsonium ion (TMI)]. This HPLC-USN-MIP-MS coupling is an encouraging combination as an alternative method for mass spectroscopy for elemental speciation analysis. Interchanging of the MIP-MS fabricated nebulizer (concentric) with an ultrasonic nebulizer, increases 3-6 times the ion signals for the anionic and 6-12 times those for the cationic arsenic compounds as compared to traditional methods. The HPLC-USN-MIP-MS combination used is excellent, amplifying the ion signals about 1.5-2 times for cationic and 1.3-3.8 times for the anionic arsenic compounds as compared to the HPLC-ICPMS coupling, The detection limits for As(V), MA, DMA, AB, TMAO, AC, and TMI (in Milli-Q-water) obtained with the optimized HPLC-USN-N-2-MIP-MS system are 0.46, 0.36, 0.73, 0.21, 3.64, 0.39, and 0.32 µg L-1, respectively, about 13-50 times lower than the HPLC-MIP-MS and about 3-11 times lower than the HPLC-ICPMS. The detection limits of As(V), MA, DMA, AB, TMAO, AC, and TMI, which spike in the urine, are deteriorated by 1.7-4.2 times compared with the detection limits of the seven different As compounds, which are prepared in the Milli-Q-water, The repeatability (RSD for three successive analyzes) and reproducibility (RSD for three successive analyzes performed on three different days), considering peak area and peak height, achieved for seven different arsenic compounds are 0.5-7 and 0.7-8%, comparable with the HPLC-ICPMS (0.3-8.5%; 4-12%) and HPLC-MIP-MS (0.4-9%; 5-12%) systems. The combined HPLC-USN-N-2-MIP-MS has been adequately applied to the determination of AB in NIES Candidate Human Urine CRM. The results agree with the HPLC-ICPMS values. Chloride interference as (ArCl+)-Ar-40-Cl-35 is not found in the urine and with the high chloride matrix (10 000 mg L-1).

"Determination Of Selenoethionine By Flow Injection-hydride Generation-atomic Absorption Spectrometry/high-performance Liquid Chromatography-hydride Generation-high Power Nitrogen Microwave-induced Plasma Mass Spectrometry"
Anal. Chim. Acta 2001 Volume 436, Issue 2 Pages 253-263
Amit Chatterjee, Y. Shibata, A. Tanaka and M. Morita

Abstract: A simple direct flow injection hydride generation atomic absorption spectrometric method was developed using sodium tetrahydroborate and hydrochloric acid for the determination of selenoethonine (Seet) that excluded any chemical pretreatment prior to hydride generation. The detection limit (3s of blank) of the method was 0.25 ng mL-1 selenium (standard solutions in Milli-Q water), The reproducibility (RSD of three analyzes performed on three different days) and the repeatability (RSD of seven successive analyzes) of the method were 9.2% for 5.05 ng mL-1 and 2.8-9.5% for 20.0-1.00 ng mL-1 of standard selenium (Milli-Q water), respectively. The calibration graph was linear up to 20.0 ng mL-1. This HG method is very promising and was successfully applied for the on-line estimation of Seet (spiked) in human urine with using high-performance liquid chromatography-hydride generation-high power nitrogen microwave-induced plasma mass spectrometry (HPLC-HG-N-2-MIP-MS). The separation was performed on a GS-220 gel-permeating column with a 25 mM tetramethylammonium hydroxide + 25 mM malonic acid buffer (pH 7.5), which showed 26-30% signal suppression due to less volatile hydride formation from Seet among the mobile phases examined. The recovery of Seet that was prepared in the above mobile phase is about 74% as that of the Seet prepared in Milli-Q water. In the PRP- x 100 anion-exchange column with the 15 mM phosphate (pH 7.0) mobile phase, Seet eluted out after 600 s keeping a broad peak with enlarging the baseline signal. The concentration of selenite found in the human urine was 3.6±0.2 µg L-1 and that agreed well with the high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) value (3.8±0.2 µg l-1).
Speciation

"Determination Of Trimethylselenonium Ion By Flow Injection Hydride Generation Atomic Absorption Spectrometry"
Anal. Chim. Acta 1999 Volume 398, Issue 2-3 Pages 273-278
Amit Chatterjee and Y. Shibata

Abstract: A simple direct flow injection hydride generation atomic absorption spectrometric method was developed using sodium tetrahydroborate and hydrochloric acid for the determination of trimethylselenonium (TmSe) iodide which excluded any chemical pretreatment prior to hydride generation. The detection limit (2s of blank) of the method was 1.0 ng mL-1 selenium and the sensitivity was 0.15 ng mL-1. The calibration graph was linear up to 30 ng mL-1. The recoveries from tap water and urine varied with dilution, being 89-95% from tap water at 1:11 dilution, and 50-58% from urine at 1:50 dilution.
Speciation

"Temporal And Organ-specific Variability Of Selenium In Marine Organisms From The Eastern Coast Of India"
Adv. Environ. Res. 2001 Volume 5, Issue 2 Pages 167-174
Amit Chatterjee, Badal Bhattacharya and Rajdulal Das

Abstract: Temporal and organ-specific variations of selenium concentration in selected coastal organisms (seagrass, bivalves and fish) were investigated in different biotopes of the deltaic Sundarbans, in the eastern coastal region of India. The bivalves and fish were obtained from local fishermen and were destined for human consumption. The samples were digested with HNO3-H2O2 and selenium was extracted from the aqueous solution with triisooctylamine and stripped with dilute hydrochloric acid. The concentration of selenium was measured by hydride generation-atomic absorption spectrometry. The results obtained were verified using inductively coupled plasma-mass spectrometric and fluorometric methods. The mean selenium concentration found in the various species ranged from 0.05 to 3.94 µg g-1 (dry wt.). It was observed that bivalves accumulated more selenium compared to fish and seagrass. The sequence of selenium levels found was, bivalves > fish > seagrass. In seagrass, the selenium concentration was higher in the roots (0.21±0.03 µg g-1; dry wt.) than the stems (0.17±0.02 µg g-1; dry wt.) and the leaves (0.11±0.01 µg g-1; dry wt.). But, in bivalves, the maximum concentration of selenium was found in the gill (3.94±0.11 µg g-1; dry wt.). The results of the analysis of variance indicated that significant differences in Se concentration were evident between seasons and organs in these species. The variations in uptake of selenium may be due to different metabolic requirements for selenium among the three species, variations in food and differences in interspecies retention and elimination mechanisms.
Selenium NIST 1566 NIST 1571 NRCC DORM-2 Spectrophotometry Method comparison