New approach of validation using internal normalization technique for quantification of related substances in raw material, intermediates and pharmaceutical substances by HPLC

Douša, Michal; Gibala, Petr; Pekárek, Tomáš

doi:10.1016/j.jpba.2015.05.015

Cited by 11 publications

(3 citation statements)

References 12 publications

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“…HPLC separates the compounds in the test sample solution through a column such that the diverse components gradually separate and peak at diverse time points, and the detector can quantify the individual components more accurately. As a high-resolution and high-sensitivity analytical technique, if the chromatographic peaks of each compound reach baseline separation, the HPLC area normalisation method can be used to verify the content determination results accuracy using diverse colorimetric methods [ 35 ]. Herein, the results of extraction and purification of total triterpenes from the Chinese herb hawthorn leaves and liquorice using sulfuric, vanillal-sulfuric, and perchloric acid methods were different from those of the HPLC area normalisation method.…”

Section: Resultsmentioning

confidence: 99%

Development of a high-speed and ultrasensitive UV/Vis-CM for detecting total triterpenes in traditional Chinese medicine and its application

Guo,

Han,

Zhang

et al. 2024

Heliyon

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Section: Resultsmentioning

confidence: 99%

Development of a high-speed and ultrasensitive UV/Vis-CM for detecting total triterpenes in traditional Chinese medicine and its application

Guo,

Han,

Zhang

et al. 2024

Heliyon

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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%

“…The method was fully validated according to ICH Q2(R1) guideline 22 in terms of linearity, limit of detection, limit of quantification, accuracy, precision, intermediate precision, and selectivity using internal normalization (IN). 23,24 The detailed procedure of IN is described in the literature. 23 3 | RESULTS AND DISCUSSION…”

Section: Evaluation and Validation Of Methodsmentioning

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

Douša

Stach

Gibala

et al. 2016

J of Separation Science

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The amino alcohols in l-valinol were effectively separated and quantified using hydrophilic interaction chromatography with fluorescence detection. The influence of the mobile phase (salt type, buffer concentration, and pH) on retention was studied. A column TSKgel amide and mobile phase consisting of 10 mM acetate buffer pH 4.0 and acetonitrile (20:80, v/v) provided well-separated symmetric peaks of analytes. Fluorescence detection was performed using postcolumn derivatization with o-phtaldialdehyde/2-mercaptoethanol at an excitation and emission wavelength of 345 and 450 nm, respectively. Simple sample pretreatment and very high sensitivity represent the main advantages of the developed method. After validation, the method was successfully applied to the analysis of commercial samples of l-valinol.

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New approach of validation using internal normalization technique for quantification of related substances in raw material, intermediates and pharmaceutical substances by HPLC

Cited by 11 publications

References 12 publications

Development of a high-speed and ultrasensitive UV/Vis-CM for detecting total triterpenes in traditional Chinese medicine and its application

Development of a high-speed and ultrasensitive UV/Vis-CM for detecting total triterpenes in traditional Chinese medicine and its application

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

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

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