Determination of five potential genotoxic impurities in dalfampridine using liquid chromatography

Mohit Jain; Vishal Srivastava; Rajesh Kumar; Vishal Dangi; S. G. Hiriyanna; Ajay Kumar; Pramod Kumar

doi:10.1016/j.jpba.2016.10.013

Determination of five potential genotoxic impurities in dalfampridine using liquid chromatography

Mohit Jain, Vishal Srivastava, Rajesh Kumar, Vishal Dangi, S. G. Hiriyanna, Ajay Kumar, Pramod Kumar

Research output: Contribution to journal › Article › peer-review

20 Scopus citations

Abstract

A sensitive and selective HPLC method was developed for identification and quantification of five Potential genotoxic impurities (PGIs) viz. Impurity-I, Impurity-II, Impurity-III, Impurity-IV and Impurity-V in Dalfampridine (Drug substance). The method utilizes Zorbax silica column (250 mm × 4.6 mm, 5.0 μm) with UV detector in HILIC (Hydrophilic Interaction Liquid Chromatography) mode for quantitation of five PGIs. It has been validated as per International Council for Harmonisation (ICH) guidelines and is able to quantitate all PGIs at 75 ppm with respect to 20 mg/mL of sample concentration. It is linear in the range of 22.5–112.5 ppm for all PGIs, which matches the range of LOQ-150% of estimated permitted level (75 ppm). Its accuracy was established in the range from 88.14 to 107.65% for these PGIs. The correlation coefficient of each impurity was >0.999. It is a good quality control tool for quantitation of PGIs in Dalfampridine at low level.

Original language	English
Pages (from-to)	27-31
Number of pages	5
Journal	Journal of Pharmaceutical and Biomedical Analysis
Volume	133
DOIs	https://doi.org/10.1016/j.jpba.2016.10.013
State	Published - 30 Jan 2017
Externally published	Yes

Bibliographical note

Publisher Copyright:
© 2016 Elsevier B.V.

Keywords

Dalfampridine
Genotoxic impurity
HILIC mode
RP-HPLC
UV detector
Validation

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10.1016/j.jpba.2016.10.013

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abstract = "A sensitive and selective HPLC method was developed for identification and quantification of five Potential genotoxic impurities (PGIs) viz. Impurity-I, Impurity-II, Impurity-III, Impurity-IV and Impurity-V in Dalfampridine (Drug substance). The method utilizes Zorbax silica column (250 mm × 4.6 mm, 5.0 μm) with UV detector in HILIC (Hydrophilic Interaction Liquid Chromatography) mode for quantitation of five PGIs. It has been validated as per International Council for Harmonisation (ICH) guidelines and is able to quantitate all PGIs at 75 ppm with respect to 20 mg/mL of sample concentration. It is linear in the range of 22.5–112.5 ppm for all PGIs, which matches the range of LOQ-150% of estimated permitted level (75 ppm). Its accuracy was established in the range from 88.14 to 107.65% for these PGIs. The correlation coefficient of each impurity was >0.999. It is a good quality control tool for quantitation of PGIs in Dalfampridine at low level.",

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author = "Mohit Jain and Vishal Srivastava and Rajesh Kumar and Vishal Dangi and Hiriyanna, {S. G.} and Ajay Kumar and Pramod Kumar",

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doi = "10.1016/j.jpba.2016.10.013",

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AU - Jain, Mohit

AU - Srivastava, Vishal

AU - Kumar, Rajesh

AU - Dangi, Vishal

AU - Hiriyanna, S. G.

AU - Kumar, Ajay

AU - Kumar, Pramod

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AB - A sensitive and selective HPLC method was developed for identification and quantification of five Potential genotoxic impurities (PGIs) viz. Impurity-I, Impurity-II, Impurity-III, Impurity-IV and Impurity-V in Dalfampridine (Drug substance). The method utilizes Zorbax silica column (250 mm × 4.6 mm, 5.0 μm) with UV detector in HILIC (Hydrophilic Interaction Liquid Chromatography) mode for quantitation of five PGIs. It has been validated as per International Council for Harmonisation (ICH) guidelines and is able to quantitate all PGIs at 75 ppm with respect to 20 mg/mL of sample concentration. It is linear in the range of 22.5–112.5 ppm for all PGIs, which matches the range of LOQ-150% of estimated permitted level (75 ppm). Its accuracy was established in the range from 88.14 to 107.65% for these PGIs. The correlation coefficient of each impurity was >0.999. It is a good quality control tool for quantitation of PGIs in Dalfampridine at low level.

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KW - RP-HPLC

KW - UV detector

KW - Validation

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Determination of five potential genotoxic impurities in dalfampridine using liquid chromatography

Abstract

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Keywords

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