ABSTRACT
OBJECTIVE: The main aim of the present work is to synthesize chloramphenicol impurity A (CLRMIMP- A) in the purest form and its subsequent characterization by using a panel of sophisticated analytical techniques (LC-MS, DSC, TGA, NMR, FTIR, HPLC, and CHNS) to provide as a reference standard mentioned in most of the international compendiums, including IP, BP, USP, and EP. The present synthetic procedure has not been disclosed anywhere in the prior art. METHODS: A simple, cheaper, and new synthesis method was described for the preparation of CLRM-IMP-A. It was synthesized and characterized by FTIR, DSC, TGA, NMR (1H and 13C), LC-MS, CHNS, and HPLC. RESULTS: CLRM-IMP-A present in drugs and dosage form can alter the therapeutic effects and adverse reaction of a drug considerably, it is mandatory to have a precise method for the estimation of impurities to safeguard the public health. Under these circumstances, the presence of CLRM-IMP-A in chloramphenicol (CLRM) requires strict quality control to satisfy the specified regulatory limit. The synthetic impurity obtained was in the pure form to provide a certified reference standard or working standard to stakeholders with defined potency. CONCLUSION: The present research describes a novel technique for the synthesis of pharmacopoeial impurity, which can help in checking/controlling the quality of the CLRM in the international markets.
Subject(s)
Chloramphenicol/analogs & derivatives , Drug Contamination/prevention & control , Chloramphenicol/analysis , Chloramphenicol/chemical synthesis , Chloramphenicol/standards , Reference StandardsSubject(s)
Adverse Drug Reaction Reporting Systems/organization & administration , Drug-Related Side Effects and Adverse Reactions , Medication Therapy Management/organization & administration , Pediatrics , Safety Management , Drug Monitoring/standards , Drug-Related Side Effects and Adverse Reactions/diagnosis , Drug-Related Side Effects and Adverse Reactions/prevention & control , Humans , India , Pediatrics/methods , Pediatrics/standards , Pharmacovigilance , Safety Management/methods , Safety Management/organization & administrationABSTRACT
A new phenolic glucoside, (rel)-2-(4',6' -dibenzoyl-beta-glucopyranosyloxy)-7-(1alpha-hydroxy-2alpha-ethoxy-6alpha-acetyloxy-3-oxocyclohex-4-enoyl)-benzyl alcohol (Flacourticin) (1) and the known, 2-(4',6'-dibenzoyl-beta-glucopyranosyl)-5-hydroxy benzyl alcohol (4'-benzoylpoliothrysoside) (2) together with the new, (2E)-heptyl-3-(3,4-dihydroxyphenyl) acrylate (3), (+)-catechin (4) and sitosterol-beta-D-glucoside were isolated from Flacourtia indica. Their structures were assigned on the basis of 1D, 2D-NMR and as well by analysis of the LC-ESIMS data. The isolated compounds (1-4) were evaluated for alpha,alpha-diphenyl-beta-picrylhydrazyl (DPPH) radical scavenging activity, and 3 was found to be two-fold less potent, with an IC50 = 12.01 microg/mL, compared to the positive control, Rutin, (IC50 = 5.83 microg/mL).
