Effect of on-capillary large volume sample stacking on limits of detection in the capillary zone electrophoretic determination of selected drugs, dyes and metal chelates

Franklin Smyth, GB Harland, Stephen McClean, G McGrath, D Oxspring

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Abstract

On-capillary large volume sample stacking (LVSS) with hydrodynamic injections of up to 240 s can be used to significantly decrease the limits of detection (LODs) of selected cationic basic drugs, such as clenbuterol, narcotine, flurazepam, codeine and pethidine, by capillary zone electrophoresis (CZE) by up to two orders of magnitude. This technique for these cations requires the use of the electroosmotic flow (EOF) modifier, cetyltrimethylammonium bromide (CTAB), employed at a concentration of 0.002 mol l(-1) in a run buffer of 0.05 mol l(-1) disodium tetraborate adjusted to pH 2.2 with orthophosphoric acid. In addition, polarity switching has to be employed after stacking and sample solvent removal in order to effect migration to the UV detector set at 210 nm. Similarily, but using visible detection and a run buffer of 0.05 mol l(-1) sodium acetate, 0.002 mol l(-1) CTAB and 1.0.10(-7) mol l(-1) of chelating agent 2-(5'-bromo-2-pyridylazo)-5-diethylamino phenol (5-Br-PADAP) at pH 8, cobalt may be determined as its cationic chelate by LVSS. An LOD of 5.10(-8) mol l(-1) cobalt can be achieved. Anionic species, such as dyes containing SO3- groups, can also be subjected to LVSS using the EOF modifier, diethylenetriamine (DETA) at a concentration of 0.006 mol l(-1) in a run electrolyte of 0.05 mol l(-1) citric acid (pH 2.23). Using a 30 s hydrodynamic injection and reversed polarity CZE without post-stacking polarity switching, LODs can be decreased by up to 20 times. The anionic chelate of boron with the ligand Azomethine H can be subjected to LVSS using the same EOF modifier and run electrolyte. A decrease in LOD is again found, down to a value of 5.10(-8) mol l(-1). This method can be applied to the selective determination of boron at realistic concentrations in an artificial river water matrix containing some 20 trace metal ions.
LanguageEnglish
Pages161-169
JournalJOURNAL OF CHROMATOGRAPHY A
Volume772
Issue number1-2
Publication statusPublished - Jun 1997

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Boron
Cobalt
Electrophoresis
Electrolytes
Buffers
Noscapine
Coloring Agents
Hydrodynamics
Metals
Flurazepam
Clenbuterol
Ultraviolet detectors
Sodium Acetate
Codeine
Meperidine
Chelating Agents
Phenol
Citric Acid
Pharmaceutical Preparations
Metal ions

Cite this

@article{e4015568f4ed4334a0c6c5571b5bafce,
title = "Effect of on-capillary large volume sample stacking on limits of detection in the capillary zone electrophoretic determination of selected drugs, dyes and metal chelates",
abstract = "On-capillary large volume sample stacking (LVSS) with hydrodynamic injections of up to 240 s can be used to significantly decrease the limits of detection (LODs) of selected cationic basic drugs, such as clenbuterol, narcotine, flurazepam, codeine and pethidine, by capillary zone electrophoresis (CZE) by up to two orders of magnitude. This technique for these cations requires the use of the electroosmotic flow (EOF) modifier, cetyltrimethylammonium bromide (CTAB), employed at a concentration of 0.002 mol l(-1) in a run buffer of 0.05 mol l(-1) disodium tetraborate adjusted to pH 2.2 with orthophosphoric acid. In addition, polarity switching has to be employed after stacking and sample solvent removal in order to effect migration to the UV detector set at 210 nm. Similarily, but using visible detection and a run buffer of 0.05 mol l(-1) sodium acetate, 0.002 mol l(-1) CTAB and 1.0.10(-7) mol l(-1) of chelating agent 2-(5'-bromo-2-pyridylazo)-5-diethylamino phenol (5-Br-PADAP) at pH 8, cobalt may be determined as its cationic chelate by LVSS. An LOD of 5.10(-8) mol l(-1) cobalt can be achieved. Anionic species, such as dyes containing SO3- groups, can also be subjected to LVSS using the EOF modifier, diethylenetriamine (DETA) at a concentration of 0.006 mol l(-1) in a run electrolyte of 0.05 mol l(-1) citric acid (pH 2.23). Using a 30 s hydrodynamic injection and reversed polarity CZE without post-stacking polarity switching, LODs can be decreased by up to 20 times. The anionic chelate of boron with the ligand Azomethine H can be subjected to LVSS using the same EOF modifier and run electrolyte. A decrease in LOD is again found, down to a value of 5.10(-8) mol l(-1). This method can be applied to the selective determination of boron at realistic concentrations in an artificial river water matrix containing some 20 trace metal ions.",
author = "Franklin Smyth and GB Harland and Stephen McClean and G McGrath and D Oxspring",
note = "10th International Symposium on Capillary Electrophoresis and Isotachophoresis (ITP 96), PRAGUE, CZECH REPUBLIC, SEP 17-20, 1996",
year = "1997",
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volume = "772",
pages = "161--169",
journal = "JOURNAL OF CHROMATOGRAPHY A",
issn = "0021-9673",
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TY - JOUR

T1 - Effect of on-capillary large volume sample stacking on limits of detection in the capillary zone electrophoretic determination of selected drugs, dyes and metal chelates

AU - Smyth, Franklin

AU - Harland, GB

AU - McClean, Stephen

AU - McGrath, G

AU - Oxspring, D

N1 - 10th International Symposium on Capillary Electrophoresis and Isotachophoresis (ITP 96), PRAGUE, CZECH REPUBLIC, SEP 17-20, 1996

PY - 1997/6

Y1 - 1997/6

N2 - On-capillary large volume sample stacking (LVSS) with hydrodynamic injections of up to 240 s can be used to significantly decrease the limits of detection (LODs) of selected cationic basic drugs, such as clenbuterol, narcotine, flurazepam, codeine and pethidine, by capillary zone electrophoresis (CZE) by up to two orders of magnitude. This technique for these cations requires the use of the electroosmotic flow (EOF) modifier, cetyltrimethylammonium bromide (CTAB), employed at a concentration of 0.002 mol l(-1) in a run buffer of 0.05 mol l(-1) disodium tetraborate adjusted to pH 2.2 with orthophosphoric acid. In addition, polarity switching has to be employed after stacking and sample solvent removal in order to effect migration to the UV detector set at 210 nm. Similarily, but using visible detection and a run buffer of 0.05 mol l(-1) sodium acetate, 0.002 mol l(-1) CTAB and 1.0.10(-7) mol l(-1) of chelating agent 2-(5'-bromo-2-pyridylazo)-5-diethylamino phenol (5-Br-PADAP) at pH 8, cobalt may be determined as its cationic chelate by LVSS. An LOD of 5.10(-8) mol l(-1) cobalt can be achieved. Anionic species, such as dyes containing SO3- groups, can also be subjected to LVSS using the EOF modifier, diethylenetriamine (DETA) at a concentration of 0.006 mol l(-1) in a run electrolyte of 0.05 mol l(-1) citric acid (pH 2.23). Using a 30 s hydrodynamic injection and reversed polarity CZE without post-stacking polarity switching, LODs can be decreased by up to 20 times. The anionic chelate of boron with the ligand Azomethine H can be subjected to LVSS using the same EOF modifier and run electrolyte. A decrease in LOD is again found, down to a value of 5.10(-8) mol l(-1). This method can be applied to the selective determination of boron at realistic concentrations in an artificial river water matrix containing some 20 trace metal ions.

AB - On-capillary large volume sample stacking (LVSS) with hydrodynamic injections of up to 240 s can be used to significantly decrease the limits of detection (LODs) of selected cationic basic drugs, such as clenbuterol, narcotine, flurazepam, codeine and pethidine, by capillary zone electrophoresis (CZE) by up to two orders of magnitude. This technique for these cations requires the use of the electroosmotic flow (EOF) modifier, cetyltrimethylammonium bromide (CTAB), employed at a concentration of 0.002 mol l(-1) in a run buffer of 0.05 mol l(-1) disodium tetraborate adjusted to pH 2.2 with orthophosphoric acid. In addition, polarity switching has to be employed after stacking and sample solvent removal in order to effect migration to the UV detector set at 210 nm. Similarily, but using visible detection and a run buffer of 0.05 mol l(-1) sodium acetate, 0.002 mol l(-1) CTAB and 1.0.10(-7) mol l(-1) of chelating agent 2-(5'-bromo-2-pyridylazo)-5-diethylamino phenol (5-Br-PADAP) at pH 8, cobalt may be determined as its cationic chelate by LVSS. An LOD of 5.10(-8) mol l(-1) cobalt can be achieved. Anionic species, such as dyes containing SO3- groups, can also be subjected to LVSS using the EOF modifier, diethylenetriamine (DETA) at a concentration of 0.006 mol l(-1) in a run electrolyte of 0.05 mol l(-1) citric acid (pH 2.23). Using a 30 s hydrodynamic injection and reversed polarity CZE without post-stacking polarity switching, LODs can be decreased by up to 20 times. The anionic chelate of boron with the ligand Azomethine H can be subjected to LVSS using the same EOF modifier and run electrolyte. A decrease in LOD is again found, down to a value of 5.10(-8) mol l(-1). This method can be applied to the selective determination of boron at realistic concentrations in an artificial river water matrix containing some 20 trace metal ions.

M3 - Article

VL - 772

SP - 161

EP - 169

JO - JOURNAL OF CHROMATOGRAPHY A

T2 - JOURNAL OF CHROMATOGRAPHY A

JF - JOURNAL OF CHROMATOGRAPHY A

SN - 0021-9673

IS - 1-2

ER -