2018
DOI: 10.1002/rcm.8151
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Liquid chromatography/electrospray ionization tandem mass spectrometry study of repaglinide and its forced degradation products

Abstract: The forced degradation of RP carried out as per ICH guidelines results in the formation of six degradation products which have been characterized using LC/MS/MS in combination with accurate mass measurements.

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Cited by 7 publications
(9 citation statements)
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“…The mass fragmentation pathway for the OXC and its corresponding DPs was established using the ESI technique in positive mode. During the sample run, the QTOF parameters, including capillary voltage, fragmentor voltage, skimmer voltage, drying gas flow, dry gas temperature, collision gas, drying gas and nebuliser gas, were optimised to enhance the intensity of the molecular ion peaks and their fragments 24 …”
Section: Methodsmentioning
confidence: 99%
“…The mass fragmentation pathway for the OXC and its corresponding DPs was established using the ESI technique in positive mode. During the sample run, the QTOF parameters, including capillary voltage, fragmentor voltage, skimmer voltage, drying gas flow, dry gas temperature, collision gas, drying gas and nebuliser gas, were optimised to enhance the intensity of the molecular ion peaks and their fragments 24 …”
Section: Methodsmentioning
confidence: 99%
“…1 H-NMR, 13 C NMR, and 2D NMR data were generated on Bruker (400 MHz) instrument under the method parameters relaxation delay (D1) = 1 s, acquisition (AQ) = 4.19 s, pulse prog = zg30, number of scans (NS) = 64 s, dwell time (DT) = 64 s, and no. of data points (TD) = 64K, with DMSO-d6 solvent.…”
Section: Instrumentation and Conditionsmentioning
confidence: 99%
“…The main aim of the present study was to establish the nature of degradation impurities that involved enrichment, isolation, and characterization of degradation impurities, and the development and validation of suitable stability-indicating analytical method. Liquid chromatography-mass spectrometry (LC-MS), high-resolution mass spectrometry (HR-MS) [9][10][11][12][13][14], and two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy [15][16][17][18][19][20][21][22] techniques have been extensively used as powerful technologies in identifying and characterizing DPs.…”
Section: Introductionmentioning
confidence: 99%
“…It is worth mentioning that none of them was documented in the pharmacopoeial monograph of repaglinide. In addition, one report from the literature [38] described the stress degradation of repaglinide and reported six degradation products (DPs 8-13). Four DPs (8)(9)(10)(11) In addition, one report from the literature [38] described the stress degradation of repaglinide and reported six degradation products (DPs 8-13).…”
Section: Identification Of Degradation Productsmentioning
confidence: 99%
“…Four DPs (8)(9)(10)(11) In addition, one report from the literature [38] described the stress degradation of repaglinide and reported six degradation products (DPs 8-13). Four DPs (8)(9)(10)(11) In addition, one report from the literature [38] described the stress degradation of repaglinide and reported six degradation products (DPs 8-13). Four DPs (8)(9)(10)(11) were formed under acidic conditions (1M HCl), two DPs (8,9) under basic conditions (1M NaOH), while three DPs (11)(12)(13) were formed under oxidative conditions (30% H 2 O 2 ).…”
Section: Identification Of Degradation Productsmentioning
confidence: 99%