TY - JOUR
T1 - Analytical methodology for the simultaneous determination of NMG-Sb(v), iSb(v), and iSb(iii) species by anion exchange liquid chromatography in Glucantime® and its biological application in Wistar rat urine
AU - Roldán, Nicole
AU - Pizarro, Danitza
AU - Frezard, Frederic
AU - BRAVO MERCADO, MANUEL ANDRES
AU - Verdugo, Marcelo
AU - Suzuki, Noriyuki
AU - Ogra, Yasumitsu
AU - Quiroz, Waldo
N1 - Publisher Copyright:
© 2019 The Royal Society of Chemistry.
Copyright:
Copyright 2019 Elsevier B.V., All rights reserved.
PY - 2019/1
Y1 - 2019/1
N2 - Several methodologies have been studied to determine the species of antimony (Sb) present in Glucantime®. However, these techniques have certain disadvantages, such as a low resolution between N-methylglucamine (NMG-Sb(v)) and inorganic pentavalent Sb (iSb(v)). Furthermore, there is a problem regarding the stability of inorganic trivalent Sb (iSb(iii)) during sample treatment. The main aim of this work was to develop an analytical methodology for the separation of the Sb species of NMG-Sb(v), iSb(v), and iSb(iii) in Glucantime®. To achieve this, a methodology was developed based on anion exchange high performance liquid chromatography hydride generation atomic fluorescence (HPLC-HG-AFS) in gradient elution mode with different concentrations of Na 2 H 2 EDTA as the mobile phase. The results show that 0.473 mM Na 2 H 2 EDTA should be used for 1.20 min as the first mobile phase for the separation of NMG-Sb(v), which should then be changed to 20 mM for the elution of the inorganic species. The results also reveal that the iSb(iii) content may be underestimated when sample filtration is used prior to the separation step. Instead of filtration, this study demonstrates that adjustment to pH 9 and dilution with deionized water are a better strategy to determine the iSb(iii) content. This method proves to be reproducible for application in urine samples from rats injected intraperitoneally with NMG-Sb(v).
AB - Several methodologies have been studied to determine the species of antimony (Sb) present in Glucantime®. However, these techniques have certain disadvantages, such as a low resolution between N-methylglucamine (NMG-Sb(v)) and inorganic pentavalent Sb (iSb(v)). Furthermore, there is a problem regarding the stability of inorganic trivalent Sb (iSb(iii)) during sample treatment. The main aim of this work was to develop an analytical methodology for the separation of the Sb species of NMG-Sb(v), iSb(v), and iSb(iii) in Glucantime®. To achieve this, a methodology was developed based on anion exchange high performance liquid chromatography hydride generation atomic fluorescence (HPLC-HG-AFS) in gradient elution mode with different concentrations of Na 2 H 2 EDTA as the mobile phase. The results show that 0.473 mM Na 2 H 2 EDTA should be used for 1.20 min as the first mobile phase for the separation of NMG-Sb(v), which should then be changed to 20 mM for the elution of the inorganic species. The results also reveal that the iSb(iii) content may be underestimated when sample filtration is used prior to the separation step. Instead of filtration, this study demonstrates that adjustment to pH 9 and dilution with deionized water are a better strategy to determine the iSb(iii) content. This method proves to be reproducible for application in urine samples from rats injected intraperitoneally with NMG-Sb(v).
UR - http://www.scopus.com/inward/record.url?scp=85059592427&partnerID=8YFLogxK
U2 - 10.1039/c8ja00273h
DO - 10.1039/c8ja00273h
M3 - Article
AN - SCOPUS:85059592427
VL - 34
SP - 203
EP - 213
JO - Journal of Analytical Atomic Spectrometry
JF - Journal of Analytical Atomic Spectrometry
SN - 0267-9477
IS - 1
ER -