Analysis of Residual Solvents-Impurities by HS-GC-FID: Case of Seven Samples of Ciprofloxacin API.

Abstract

Residual solvents are organic volatile impurities that can occur in the manufacture of Active Pharmaceutical Ingredients (APIs). Residual solvents analysis in pharmaceutical products is necessary not only because of they represent a potential risk for human health due to their toxicity and their undesirables side effects, but also because they may affect the physicochemical proprieties of pharmaceutical product. The main objective of this work was to analysis 29 residual solvents-impurities by Head Space Gas Chromatography with Flame Ionization Detector (HS-GC-FID) in seven samples of Ciprofloxacin Hydrochloride API, collected from seven pharmaceutical industries installed in Algeria. The GC was equipped with a flame-ionization detector and silica column coated with 1.8 µm layer of phase G43. The carrier gas was helium with a linear velocity of 35 cm/s and a split ratio of 1:5. The column temperature was 40 °C then it rised to 240 °C. The injection temperature was 140 °C and that of detector was 250 °C. Twenty-nine organic solvents belong to classes 1 and 2 were analyzed in seven samples of Ciprofloxacin Hydrochloride API whose control is mandatory because of their carcinogenic and intrinsic toxicity. Only five solvents were identified wich are Hexane, Toluene, Acetonitrile, Methanol and Dichloromethane in the different samples. All samples collected satisfied the test of identification, so, the confirmation and the quantification procedures weren’t realized. The HS-GC-FID technique used showed that the identified solvents differ from one sample to another of the same molecule. This showed that manufacturers didn’t often use the same solvents to produce the same API, which justifies that residual organic solvent tests weren’t usually mentioned in the specific monographs.