Quantification of structurally related aliphatic amino alcohols in <scp>l‐</scp>valinol by hydrophilic interaction liquid chromatography separation combined with postcolumn derivatization and fluorescence detection

Douša, Michal; Stach, Jan; Gibala, Petr; Lemr, Karel

doi:10.1002/jssc.201501302

Cited by 9 publications

(12 citation statements)

References 23 publications

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“…The influence of flow rate of derivatization reagent , the derivatization reagent concentration and pH , temperature of derivatization reaction , and finally the volume of capillary coil reactor on the fluorescence detector response have been investigated for the conditions of postcolumn derivatization. The influence of the molecular structure on detector response during derivatization reaction of amines with OPA has already been shortly discussed . The response factors (RF) of tested compounds related to methylamine or cyclobutylamine were determined using the following equation:

R F = (\frac{A_{REF}}{c_{REF}} \frac{c_{DET}}{A_{DET}})

where A REF stands for response of reference compound, A DET is response of a tested compound, c REF is concentration of reference compound, and c DET is concentration of a tested compound.…”

Section: Resultsmentioning

confidence: 99%

“…In the literature, it was shown that the application of postcolumn derivatization is more suitable due to simplicity and instability of the OPA fluorescent derivatives . The influence of flow rate of derivatization reagent , the derivatization reagent concentration , buffer pH , temperature of derivatization reaction , and finally the volume of capillary coil reactor on detector response have been investigated for the conditions of postcolumn derivatization.…”

Section: Introductionmentioning

confidence: 99%

“…In the literature, it was shown that the application of postcolumn derivatization is more suitable due to simplicity and instability of the OPA fluorescent derivatives [3]. The influence of flow rate of derivatization reagent [3,4], the derivatization reagent concentration [5,6], buffer pH [3], temperature of derivatization reaction [5], and finally the volume of capillary coil reactor [3] on detector response have been investigated for the conditions of postcolumn derivatization.Analysis of volatile amines is difficult because of their high volatility, polarity, basic character, and lack of How to cite this article: Douša M, Doubský J. Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o-phthaldialdehyde/mercaptoethanol.…”

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confidence: 99%

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Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o‐phthaldialdehyde/mercaptoethanol

Douša

Doubský

2017

J of Separation Science

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The retention behavior of primary aliphatic amines (homologous series of aliphatic alkyl amines and cycloalkyl amines) and positional isomers of alkylamines in the hydrophilic interaction chromatography mode was studied. The study was carried out on a TSKgel Amide-80 column followed by postcolumn derivatization with fluorescence detection to describe the retention mechanism of tested compounds. The effect of chromatographic conditions including column temperature, acetonitrile content in the mobile phase, mobile phase pH (ranging from 3.5 to 6.8), and salt concentration in the mobile phase was investigated. The final mobile phase consisted of acetonitrile and solution of 20 mM potassium formate pH 3.5 in ratio 80:20 v/v. The analyses were carried out at mobile phase flow rate of 1.0 mL/min and the column temperature of 20°C. The developed method was fully validated in terms of linearity, sensitivity (limit of detection and limit of quantification), accuracy, and precision according to International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. The proposed new methods were proved to be highly sensitive, simple, and rapid, and were successfully applied to the determinations of isopropylamine, cyclohexylamine, and cyclopropylamine in relevant active pharmaceutical ingredients.

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R F = (\frac{A_{REF}}{c_{REF}} \frac{c_{DET}}{A_{DET}})

where A REF stands for response of reference compound, A DET is response of a tested compound, c REF is concentration of reference compound, and c DET is concentration of a tested compound.…”

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o‐phthaldialdehyde/mercaptoethanol

Douša

Doubský

2017

J of Separation Science

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“…23,24 The detailed procedure of IN is described in the literature. The final chromatographic conditions were optimized to obtain retention factor k ≥ 2, efficiency N ≥ 6000 for first eluting enantiomer and to achieve baseline separation (resolution R S ≥ 2.0).…”

Section: Evaluation and Validation Of Methodsmentioning

confidence: 99%

“…24 The sample solutions of L-Valinol at concentration of 10 μg/mL with different additions of D-Valinol (the concentration range from LOQ to 200% of the target specification limit with respect to L-Valinol sample solution, the 100% specification limit corresponded to 0.015 μg/mL) were prepared. 24 The sample solutions of L-Valinol at concentration of 10 μg/mL with different additions of D-Valinol (the concentration range from LOQ to 200% of the target specification limit with respect to L-Valinol sample solution, the 100% specification limit corresponded to 0.015 μg/mL) were prepared.…”

Section: Limit Of Detection and Quantification Accuracy And Lineamentioning

confidence: 99%

Chiral separation of aliphatic primary amino alcohols as o‐phthaldialdehyde/mercaptoethanol derivatives on polysaccharide‐based chiral stationary phases

Douša¹

2019

Chirality

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A sensitive chiral high performance liquid chromatography (HPLC) method for the determination of aliphatic primary amino alcohol isomers with ophthaldialdehyde/mercaptoethanol precolumn derivatization has been developed and validated. Seven chiral columns were tested in a reversed phase mode. Excellent enantioseparation with the resolution more than 2.0 was achieved on Chiralcel OJ-3R. The effect of various chromatographic conditions including column temperature, acetonitrile content in the mobile phase, buffer pH, buffer concentration, and buffer type in the mobile phase on the retention and the selectivity was investigated. The final mobile phase consisted of binary mixture of 20mM ammonium formate solution with acetonitrile (75:25; v/v).The analyses were performed at mobile phase flow rate of 1.0 mL/min and the column temperature of 40°C. The fluorescence detection was performed at excitation wavelength of 345 nm and emission wavelength of 450 nm. The developed method was fully validated in terms of linearity, sensitivity, accuracy, precision, intermediate precision, and selectivity according to International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines using internal normalization procedure. The proposed chiral method was proved to be highly sensitive, simple, and rapid and was successfully applied to the determination of D-Valinol content in commercially available samples of L-Valinol.

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Optimization of o‐phtaldialdehyde/2‐mercaptoethanol postcolumn reaction for the hydrophilic interaction liquid chromatography determination of memantine utilizing a silica hydride stationary phase

Douša

Pivoňková

Sýkora

2016

J of Separation Science

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A rapid procedure for the determination of memantine based on hydrophilic interaction chromatography with fluorescence detection was developed. Fluorescence detection after postcolumn derivatization with o-phtaldialdehyde/2-mercaptoethanol was performed at excitation and emission wavelengths of 345 and 450 nm, respectively. The postcolumn reaction conditions such as reaction temperature, derivatization reagent flow rate, and reagents concentration were studied due to steric hindrance of amino group of memantine. The derivatization reaction was applied for the hydrophilic interaction liquid chromatography method which was based on Cogent Silica-C stationary phase with a mobile phase consisting of a mixture of 10 mmol/L citric acid and 10 mmol/L o-phosphoric acid (pH 6.0) with acetonitrile using an isocratic composition of 2:8 v/v. The benefit of the reported approach consists in a simple sample pretreatment and a quick and sensitive hydrophilic interaction chromatography method. The developed method was validated in terms of linearity, accuracy, precision, and selectivity according to the International Conference on Harmonisation guidelines. The developed method was successfully applied for the analysis of commercial memantine tablets.

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Quantification of structurally related aliphatic amino alcohols in l‐valinol by hydrophilic interaction liquid chromatography separation combined with postcolumn derivatization and fluorescence detection

Cited by 9 publications

References 23 publications

Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o‐phthaldialdehyde/mercaptoethanol

Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o‐phthaldialdehyde/mercaptoethanol

Chiral separation of aliphatic primary amino alcohols as o‐phthaldialdehyde/mercaptoethanol derivatives on polysaccharide‐based chiral stationary phases

Optimization of o‐phtaldialdehyde/2‐mercaptoethanol postcolumn reaction for the hydrophilic interaction liquid chromatography determination of memantine utilizing a silica hydride stationary phase

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