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

Abstract

Organic volatile impurities known as residual solvents might appear during the production of active pharmaceutical ingredients (APIs). Analysis of residual solvents in pharmaceutical products is necessary due to the potential risk they provide to human health due to their toxicity and unfavorable side effects, as well as the possibility that they may change the physicochemical properties of the pharmaceutical product. The goal of this study was to analysis 29 residual solvents-impurities using Head Space Gas Chromatography with Flame Ionization Detector (HS-GC-FID) in seven Ciprofloxacin Hydrochloride API samples that were gathered from seven pharmaceutical companies located in Algeria. A flame-ionization detector and a silica column covered with a 1.8 m layer of phase G43 were both installed in the GC. Helium served as the carrier gas, having a split ratio of 1:5 and a linear velocity of 35 cm/s. The temperature of the column began at 40 °C and increased to 240 °C. The temperature of the injection was 140 °C, while the detector temperature 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.

Keywords

• Residual solvents
• Solvents-impurties
• Ciprofloxacin Hydrochloride
• Fluoroquinolone
• Antibiotic
• HS-GC-FID

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